# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

loop_
_publ_author_name
'Yaoyu Feng'
'Jiangyong Hu'
'Wun-Jern Ng'
'Say-Leong Ong'
;
Zhiming Wang
;
'Xinhua Zhong'

_publ_contact_author_name        'Dr Yaoyu Feng'
_publ_contact_author_address     
;
Dept of Civil Engineering, Natioanl
Singapore
SINGAPORE
;

_publ_contact_author_email       CVEFYY@NUS.EDU.SG

_publ_section_title              
;
Strong optical limiting capability of a triosmium
cluster bonded indium porphyrin complex [(TPP)InOs3(H)2(CO)9(C5H4N)]
;

data_2
_database_code_CSD               209027

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C61.50 H34 In N5 O9 Os3'
_chemical_formula_weight         1672.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.210(2)
_cell_length_b                   13.470(3)
_cell_length_c                   18.740(4)
_cell_angle_alpha                95.22(3)
_cell_angle_beta                 99.08(3)
_cell_angle_gamma                95.24(3)
_cell_volume                     3013.3(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.39
_cell_measurement_theta_max      27.44

_exptl_crystal_description       ?
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1574
_exptl_absorpt_coefficient_mu    6.740
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.273832
_exptl_absorpt_correction_T_max  0.653827
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19302
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.39
_diffrn_reflns_theta_max         27.44
_reflns_number_total             13496
_reflns_number_gt                10688
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Siemens XSCANS'
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+9.9096P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13496
_refine_ls_number_parameters     713
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.1048
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.70402(2) 0.576801(19) 0.233643(13) 0.03587(7) Uani 1 1 d . . .
Os2 Os 0.74746(2) 0.616593(19) 0.398922(13) 0.03569(7) Uani 1 1 d . . .
Os3 Os 0.52559(2) 0.57485(2) 0.332403(13) 0.04263(8) Uani 1 1 d . . .
In In 0.90193(3) 0.59318(3) 0.18473(2) 0.03079(10) Uani 1 1 d . . .
N1 N 0.9452(4) 0.4450(4) 0.1430(3) 0.0356(11) Uani 1 1 d . . .
N2 N 1.0472(4) 0.5840(4) 0.2682(3) 0.0342(11) Uani 1 1 d . . .
N3 N 0.9694(5) 0.7519(4) 0.1943(3) 0.0395(12) Uani 1 1 d . . .
N4 N 0.8714(5) 0.6121(4) 0.0679(3) 0.0370(11) Uani 1 1 d . . .
C501 C 0.5886(5) 0.4396(5) 0.3612(3) 0.0374(14) Uani 1 1 d . . .
C1 C 0.8895(5) 0.3916(5) 0.0794(3) 0.0392(14) Uani 1 1 d . . .
C2 C 0.8968(6) 0.2872(5) 0.0831(4) 0.0487(17) Uani 1 1 d . . .
H2A H 0.8647 0.2353 0.0477 0.058 Uiso 1 1 calc R . .
C3 C 0.9593(6) 0.2779(5) 0.1481(4) 0.0501(17) Uani 1 1 d . . .
H3A H 0.9795 0.2183 0.1650 0.060 Uiso 1 1 calc R . .
C4 C 0.9888(5) 0.3766(5) 0.1862(3) 0.0365(13) Uani 1 1 d . . .
C5 C 1.0512(5) 0.4005(5) 0.2563(3) 0.0382(14) Uani 1 1 d . . .
C6 C 1.0805(5) 0.4964(5) 0.2926(3) 0.0355(13) Uani 1 1 d . . .
C7 C 1.1572(6) 0.5210(5) 0.3596(4) 0.0444(15) Uani 1 1 d . . .
H7A H 1.1929 0.4756 0.3872 0.053 Uiso 1 1 calc R . .
C8 C 1.1683(6) 0.6211(5) 0.3756(4) 0.0429(15) Uani 1 1 d . . .
H8A H 1.2124 0.6576 0.4162 0.051 Uiso 1 1 calc R . .
C9 C 1.1000(5) 0.6611(5) 0.3187(3) 0.0366(13) Uani 1 1 d . . .
C10 C 1.0882(6) 0.7641(5) 0.3149(4) 0.0420(15) Uani 1 1 d . . .
C11 C 1.0281(6) 0.8046(5) 0.2570(4) 0.0422(15) Uani 1 1 d . . .
C12 C 1.0243(7) 0.9109(5) 0.2506(4) 0.0551(19) Uani 1 1 d . . .
H12A H 1.0566 0.9634 0.2853 0.066 Uiso 1 1 calc R . .
C13 C 0.9653(8) 0.9191(5) 0.1849(4) 0.060(2) Uani 1 1 d . . .
H13A H 0.9496 0.9787 0.1661 0.072 Uiso 1 1 calc R . .
C14 C 0.9304(6) 0.8199(5) 0.1487(4) 0.0428(15) Uani 1 1 d . . .
C15 C 0.8698(7) 0.7961(5) 0.0780(4) 0.0486(17) Uani 1 1 d . . .
C16 C 0.8475(7) 0.7010(5) 0.0407(3) 0.0472(17) Uani 1 1 d . . .
C17 C 0.7921(8) 0.6773(6) -0.0339(4) 0.062(2) Uani 1 1 d . . .
H17A H 0.7673 0.7232 -0.0654 0.075 Uiso 1 1 calc R . .
C18 C 0.7829(8) 0.5786(6) -0.0494(4) 0.060(2) Uani 1 1 d . . .
H18A H 0.7509 0.5430 -0.0938 0.072 Uiso 1 1 calc R . .
C19 C 0.8307(6) 0.5366(5) 0.0138(3) 0.0399(14) Uani 1 1 d . . .
C20 C 0.8342(6) 0.4337(5) 0.0199(3) 0.0402(14) Uani 1 1 d . . .
C101 C 1.0897(6) 0.3145(5) 0.2948(4) 0.0464(16) Uani 1 1 d . . .
C102 C 1.1738(8) 0.2610(6) 0.2750(6) 0.071(2) Uani 1 1 d . . .
H10A H 1.2092 0.2796 0.2370 0.085 Uiso 1 1 calc R . .
C103 C 1.2053(10) 0.1815(8) 0.3104(8) 0.099(4) Uani 1 1 d . . .
H10B H 1.2607 0.1456 0.2954 0.118 Uiso 1 1 calc R . .
C104 C 1.1577(13) 0.1540(8) 0.3666(7) 0.106(5) Uani 1 1 d . . .
H10C H 1.1815 0.1006 0.3909 0.128 Uiso 1 1 calc R . .
C105 C 1.0735(13) 0.2050(9) 0.3881(7) 0.108(5) Uani 1 1 d . . .
H10D H 1.0387 0.1855 0.4261 0.130 Uiso 1 1 calc R . .
C106 C 1.0420(9) 0.2847(7) 0.3526(5) 0.075(3) Uani 1 1 d . . .
H10E H 0.9865 0.3201 0.3679 0.089 Uiso 1 1 calc R . .
C111 C 0.7079(7) 0.7209(6) 0.2280(4) 0.0549(19) Uani 1 1 d . . .
C112 C 0.6358(6) 0.5516(7) 0.1341(4) 0.057(2) Uani 1 1 d . . .
C113 C 0.7329(6) 0.4376(5) 0.2381(4) 0.0489(17) Uani 1 1 d . . .
C201 C 1.1506(6) 0.8348(5) 0.3769(4) 0.0433(15) Uani 1 1 d . . .
C202 C 1.1007(8) 0.8727(6) 0.4323(4) 0.061(2) Uani 1 1 d . . .
H20A H 1.0247 0.8565 0.4311 0.074 Uiso 1 1 calc R . .
C203 C 1.1629(10) 0.9354(7) 0.4905(5) 0.078(3) Uani 1 1 d . . .
H20B H 1.1275 0.9593 0.5280 0.093 Uiso 1 1 calc R . .
C204 C 1.2707(9) 0.9622(6) 0.4943(5) 0.075(3) Uani 1 1 d . . .
H20C H 1.3100 1.0056 0.5333 0.091 Uiso 1 1 calc R . .
C205 C 1.3237(9) 0.9251(8) 0.4399(6) 0.092(3) Uani 1 1 d . . .
H20D H 1.3999 0.9418 0.4425 0.111 Uiso 1 1 calc R . .
C206 C 1.2630(7) 0.8617(7) 0.3802(5) 0.077(3) Uani 1 1 d . . .
H20E H 1.2989 0.8378 0.3429 0.093 Uiso 1 1 calc R . .
C221 C 0.7697(7) 0.7599(6) 0.3946(4) 0.0537(18) Uani 1 1 d . . .
C222 C 0.8970(6) 0.6087(6) 0.4432(4) 0.0487(17) Uani 1 1 d . . .
C223 C 0.6936(6) 0.6358(5) 0.4887(4) 0.0476(16) Uani 1 1 d . . .
C301 C 0.8277(8) 0.8819(5) 0.0390(4) 0.057(2) Uani 1 1 d . . .
C302 C 0.7409(11) 0.9276(8) 0.0602(6) 0.095(4) Uani 1 1 d . . .
H30A H 0.7103 0.9068 0.0994 0.114 Uiso 1 1 calc R . .
C303 C 0.6981(15) 1.0041(9) 0.0242(7) 0.123(6) Uani 1 1 d . . .
H30B H 0.6367 1.0320 0.0379 0.148 Uiso 1 1 calc R . .
C304 C 0.7443(14) 1.0388(8) -0.0305(7) 0.111(5) Uani 1 1 d . . .
H30C H 0.7165 1.0917 -0.0536 0.133 Uiso 1 1 calc R . .
C305 C 0.8310(13) 0.9960(10) -0.0513(7) 0.114(5) Uani 1 1 d . . .
H30D H 0.8617 1.0198 -0.0897 0.136 Uiso 1 1 calc R . .
C306 C 0.8777(10) 0.9162(8) -0.0173(6) 0.089(3) Uani 1 1 d . . .
C331 C 0.5107(7) 0.7143(7) 0.3220(4) 0.061(2) Uani 1 1 d . . .
C332 C 0.3910(7) 0.5177(8) 0.2700(4) 0.066(2) Uani 1 1 d . . .
C333 C 0.4605(6) 0.5826(6) 0.4184(4) 0.0488(17) Uani 1 1 d . . .
C401 C 0.7687(6) 0.3619(5) -0.0416(4) 0.0462(16) Uani 1 1 d . . .
C402 C 0.8201(9) 0.3157(8) -0.0940(5) 0.082(3) Uani 1 1 d . . .
H40A H 0.8967 0.3299 -0.0918 0.098 Uiso 1 1 calc R . .
C403 C 0.7605(12) 0.2492(8) -0.1495(5) 0.103(4) Uani 1 1 d . . .
H40B H 0.7967 0.2180 -0.1840 0.124 Uiso 1 1 calc R . .
C404 C 0.6493(10) 0.2295(7) -0.1539(5) 0.079(3) Uani 1 1 d . . .
H40C H 0.6086 0.1852 -0.1918 0.095 Uiso 1 1 calc R . .
C405 C 0.5977(10) 0.2731(9) -0.1041(8) 0.115(5) Uani 1 1 d . . .
H40D H 0.5212 0.2581 -0.1067 0.138 Uiso 1 1 calc R . .
C406 C 0.6579(8) 0.3411(8) -0.0480(6) 0.092(4) Uani 1 1 d . . .
H40E H 0.6204 0.3726 -0.0143 0.110 Uiso 1 1 calc R . .
N5 N 0.6967(5) 0.4613(4) 0.3937(3) 0.0479(14) Uani 1 1 d . . .
O11 O 0.7098(7) 0.8023(5) 0.2224(4) 0.085(2) Uani 1 1 d . . .
O12 O 0.5957(5) 0.5383(6) 0.0751(3) 0.087(2) Uani 1 1 d . . .
O13 O 0.7552(6) 0.3581(4) 0.2403(4) 0.0792(19) Uani 1 1 d . . .
O21 O 0.7824(7) 0.8430(4) 0.3924(4) 0.089(2) Uani 1 1 d . . .
O22 O 0.9853(5) 0.6075(6) 0.4745(3) 0.084(2) Uani 1 1 d . . .
O23 O 0.6643(5) 0.6487(5) 0.5432(3) 0.0719(17) Uani 1 1 d . . .
O31 O 0.5054(7) 0.7973(6) 0.3200(4) 0.091(2) Uani 1 1 d . . .
O32 O 0.3123(5) 0.4851(7) 0.2311(3) 0.102(3) Uani 1 1 d . . .
O33 O 0.4206(5) 0.5858(5) 0.4689(3) 0.0735(18) Uani 1 1 d . . .
C505 C 0.7552(7) 0.3860(6) 0.4200(4) 0.0565(19) Uani 1 1 d . . .
C502 C 0.5397(8) 0.3445(7) 0.3548(5) 0.070(2) Uani 1 1 d . . .
H50A H 0.4653 0.3303 0.3332 0.084 Uiso 1 1 calc R . .
C504 C 0.7048(9) 0.2893(7) 0.4120(5) 0.072(3) Uani 1 1 d . . .
H50B H 0.7446 0.2381 0.4290 0.087 Uiso 1 1 calc R . .
C503 C 0.5978(10) 0.2687(7) 0.3794(6) 0.083(3) Uani 1 1 d . . .
H50C H 0.5634 0.2033 0.3737 0.100 Uiso 1 1 calc R . .
C602 C 0.628(2) 0.1216(17) 0.2033(12) 0.094(7) Uiso 0.50 1 d PD . .
H60D H 0.6880 0.1601 0.1908 0.112 Uiso 0.50 1 calc PR . .
C603 C 0.671(2) 0.0625(17) 0.2474(13) 0.103(7) Uiso 0.50 1 d PD . .
H60A H 0.7450 0.0516 0.2627 0.123 Uiso 0.50 1 calc PR . .
C604 C 0.581(2) 0.024(2) 0.2636(15) 0.108(8) Uiso 0.50 1 d PD . .
H60E H 0.5876 -0.0236 0.2967 0.130 Uiso 0.50 1 calc PR . .
C605 C 0.482(2) 0.042(2) 0.2393(17) 0.138(11) Uiso 0.50 1 d PD . .
H60B H 0.4223 0.0097 0.2565 0.166 Uiso 0.50 1 calc PR . .
C601 C 0.541(2) 0.151(2) 0.1690(16) 0.117(9) Uiso 0.50 1 d PD . .
C606 C 0.461(3) 0.105(2) 0.1921(17) 0.137(11) Uiso 0.50 1 d PD . .
H60C H 0.3875 0.1161 0.1750 0.164 Uiso 0.50 1 calc PR . .
C607 C 0.483(3) 0.214(3) 0.126(2) 0.175(15) Uiso 0.50 1 d P . .
H60F H 0.5348 0.2559 0.1050 0.263 Uiso 0.50 1 calc PR . .
H60G H 0.4435 0.2552 0.1552 0.263 Uiso 0.50 1 calc PR . .
H60H H 0.4314 0.1743 0.0880 0.263 Uiso 0.50 1 calc PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os1 0.03186(13) 0.04924(15) 0.02686(12) 0.00066(10) 0.00480(9) 0.00985(10)
Os2 0.03045(13) 0.04699(14) 0.02792(12) -0.00070(10) 0.00058(9) 0.00730(10)
Os3 0.02746(13) 0.07088(19) 0.02931(13) 0.00137(11) 0.00317(10) 0.01073(11)
In 0.0324(2) 0.0342(2) 0.0254(2) 0.00184(15) 0.00311(16) 0.00633(16)
N1 0.038(3) 0.036(3) 0.031(3) -0.001(2) 0.002(2) 0.010(2)
N2 0.034(3) 0.035(3) 0.032(3) 0.003(2) 0.002(2) 0.002(2)
N3 0.045(3) 0.039(3) 0.032(3) 0.006(2) -0.003(2) 0.003(2)
N4 0.048(3) 0.036(3) 0.027(3) 0.003(2) 0.004(2) 0.007(2)
C501 0.028(3) 0.050(4) 0.034(3) 0.000(3) 0.009(3) -0.001(3)
C1 0.039(3) 0.045(3) 0.032(3) -0.001(3) 0.004(3) 0.007(3)
C2 0.055(4) 0.036(3) 0.049(4) -0.008(3) -0.002(3) 0.006(3)
C3 0.058(5) 0.037(3) 0.051(4) -0.003(3) -0.001(4) 0.012(3)
C4 0.039(3) 0.040(3) 0.031(3) -0.001(2) 0.005(3) 0.012(3)
C5 0.034(3) 0.042(3) 0.038(3) 0.005(3) 0.003(3) 0.009(3)
C6 0.030(3) 0.040(3) 0.034(3) 0.000(2) -0.002(2) 0.007(2)
C7 0.045(4) 0.051(4) 0.035(3) 0.003(3) -0.004(3) 0.016(3)
C8 0.038(3) 0.047(4) 0.040(4) -0.001(3) -0.004(3) 0.005(3)
C9 0.038(3) 0.041(3) 0.030(3) -0.001(2) 0.004(3) 0.005(3)
C10 0.039(4) 0.045(4) 0.038(3) -0.004(3) 0.000(3) 0.005(3)
C11 0.048(4) 0.041(3) 0.035(3) 0.000(3) 0.002(3) 0.002(3)
C12 0.073(5) 0.036(4) 0.048(4) -0.003(3) -0.009(4) 0.005(3)
C13 0.086(6) 0.033(4) 0.056(5) 0.009(3) -0.002(4) 0.005(4)
C14 0.052(4) 0.037(3) 0.037(3) 0.005(3) 0.000(3) 0.007(3)
C15 0.064(5) 0.041(4) 0.039(4) 0.014(3) 0.000(3) 0.002(3)
C16 0.068(5) 0.043(4) 0.030(3) 0.008(3) 0.005(3) 0.001(3)
C17 0.093(7) 0.051(4) 0.037(4) 0.011(3) -0.010(4) 0.006(4)
C18 0.088(6) 0.056(5) 0.029(3) 0.001(3) -0.010(4) 0.008(4)
C19 0.049(4) 0.044(3) 0.025(3) 0.002(2) 0.002(3) 0.006(3)
C20 0.040(4) 0.045(4) 0.032(3) -0.005(3) 0.003(3) 0.004(3)
C101 0.054(4) 0.039(3) 0.043(4) 0.005(3) -0.007(3) 0.008(3)
C102 0.074(6) 0.058(5) 0.084(6) 0.007(4) 0.008(5) 0.028(4)
C103 0.103(9) 0.066(6) 0.123(10) 0.014(6) -0.019(8) 0.047(6)
C104 0.144(12) 0.052(6) 0.097(9) 0.020(6) -0.065(9) 0.007(7)
C105 0.147(12) 0.080(7) 0.089(8) 0.045(6) -0.016(8) -0.016(8)
C106 0.094(7) 0.062(5) 0.067(6) 0.015(4) 0.008(5) 0.009(5)
C111 0.068(5) 0.060(5) 0.045(4) 0.011(3) 0.022(4) 0.029(4)
C112 0.042(4) 0.090(6) 0.037(4) -0.009(4) 0.001(3) 0.017(4)
C113 0.052(4) 0.046(4) 0.051(4) -0.001(3) 0.021(3) 0.006(3)
C201 0.051(4) 0.040(3) 0.036(3) -0.003(3) -0.001(3) 0.008(3)
C202 0.070(6) 0.063(5) 0.047(4) -0.007(4) 0.011(4) -0.004(4)
C203 0.113(9) 0.069(6) 0.041(4) -0.016(4) 0.004(5) -0.008(5)
C204 0.098(8) 0.056(5) 0.056(5) -0.016(4) -0.031(5) 0.018(5)
C205 0.056(6) 0.096(7) 0.103(8) -0.022(6) -0.028(6) 0.000(5)
C206 0.049(5) 0.091(7) 0.080(6) -0.036(5) 0.005(4) 0.001(4)
C221 0.052(4) 0.061(5) 0.044(4) -0.007(3) 0.004(3) 0.005(4)
C222 0.039(4) 0.074(5) 0.034(3) 0.004(3) 0.008(3) 0.009(3)
C223 0.041(4) 0.059(4) 0.040(4) 0.001(3) 0.002(3) 0.010(3)
C301 0.079(6) 0.040(4) 0.045(4) 0.010(3) -0.015(4) 0.004(4)
C302 0.143(11) 0.077(7) 0.070(6) 0.016(5) 0.005(7) 0.054(7)
C303 0.196(16) 0.090(8) 0.086(8) 0.017(7) -0.007(9) 0.075(9)
C304 0.166(14) 0.062(6) 0.088(9) 0.024(6) -0.044(9) 0.021(7)
C305 0.129(12) 0.094(9) 0.110(10) 0.065(8) -0.020(9) -0.010(8)
C306 0.097(8) 0.084(7) 0.081(7) 0.050(6) -0.013(6) -0.010(6)
C331 0.054(5) 0.084(6) 0.049(4) 0.006(4) 0.011(4) 0.028(4)
C332 0.042(4) 0.123(8) 0.030(4) -0.003(4) 0.007(3) 0.008(4)
C333 0.034(4) 0.077(5) 0.035(4) 0.004(3) 0.002(3) 0.016(3)
C401 0.059(5) 0.044(4) 0.032(3) -0.002(3) -0.003(3) 0.008(3)
C402 0.091(7) 0.093(7) 0.056(5) -0.025(5) 0.032(5) -0.022(6)
C403 0.142(12) 0.100(8) 0.053(6) -0.033(5) 0.024(7) -0.036(8)
C404 0.111(9) 0.060(5) 0.049(5) -0.012(4) -0.031(5) 0.005(5)
C405 0.060(7) 0.111(9) 0.146(12) -0.049(8) -0.035(7) 0.011(6)
C406 0.055(6) 0.096(7) 0.107(8) -0.060(6) -0.002(5) 0.012(5)
N5 0.053(4) 0.055(3) 0.037(3) 0.001(3) 0.013(3) 0.007(3)
O11 0.130(6) 0.053(4) 0.089(5) 0.023(3) 0.042(4) 0.043(4)
O12 0.068(4) 0.152(7) 0.035(3) -0.013(3) -0.010(3) 0.035(4)
O13 0.103(5) 0.048(3) 0.096(5) 0.006(3) 0.046(4) 0.009(3)
O21 0.123(6) 0.042(3) 0.099(5) -0.002(3) 0.015(5) 0.002(3)
O22 0.033(3) 0.151(6) 0.065(4) 0.019(4) -0.010(3) 0.018(3)
O23 0.064(4) 0.109(5) 0.040(3) -0.013(3) 0.016(3) 0.001(3)
O31 0.094(5) 0.089(5) 0.100(5) 0.025(4) 0.020(4) 0.047(4)
O32 0.040(3) 0.202(8) 0.050(4) -0.016(4) -0.005(3) -0.019(4)
O33 0.052(3) 0.133(6) 0.041(3) 0.007(3) 0.019(3) 0.021(3)
C505 0.067(5) 0.057(5) 0.051(4) 0.019(4) 0.014(4) 0.019(4)
C502 0.065(6) 0.075(6) 0.064(5) -0.008(4) 0.013(4) -0.010(5)
C504 0.097(8) 0.056(5) 0.074(6) 0.012(4) 0.034(6) 0.026(5)
C503 0.104(9) 0.045(5) 0.100(8) -0.004(5) 0.025(7) 0.001(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C112 1.905(7) . ?
Os1 C113 1.946(7) . ?
Os1 C111 1.950(8) . ?
Os1 In 2.7142(8) . ?
Os1 Os2 3.0479(8) . ?
Os1 Os3 3.0730(9) . ?
Os2 C222 1.900(7) . ?
Os2 C223 1.905(7) . ?
Os2 C221 1.936(9) . ?
Os2 N5 2.116(6) . ?
Os2 Os3 2.7816(9) . ?
Os3 C333 1.905(7) . ?
Os3 C332 1.913(8) . ?
Os3 C331 1.928(10) . ?
Os3 C501 2.123(7) . ?
In N2 2.192(5) . ?
In N3 2.200(5) . ?
In N4 2.205(5) . ?
In N1 2.217(5) . ?
N1 C4 1.371(8) . ?
N1 C1 1.377(8) . ?
N2 C6 1.376(8) . ?
N2 C9 1.377(8) . ?
N3 C11 1.373(8) . ?
N3 C14 1.375(8) . ?
N4 C19 1.368(8) . ?
N4 C16 1.380(8) . ?
C501 C502 1.349(11) . ?
C501 N5 1.357(9) . ?
C1 C20 1.403(9) . ?
C1 C2 1.425(9) . ?
C2 C3 1.354(10) . ?
C3 C4 1.437(9) . ?
C4 C5 1.404(9) . ?
C5 C6 1.392(9) . ?
C5 C101 1.493(9) . ?
C6 C7 1.435(9) . ?
C7 C8 1.345(9) . ?
C8 C9 1.423(9) . ?
C9 C10 1.416(9) . ?
C10 C11 1.394(9) . ?
C10 C201 1.491(9) . ?
C11 C12 1.452(9) . ?
C12 C13 1.343(11) . ?
C13 C14 1.437(9) . ?
C14 C15 1.406(9) . ?
C15 C16 1.385(10) . ?
C15 C301 1.509(10) . ?
C16 C17 1.447(10) . ?
C17 C18 1.326(11) . ?
C18 C19 1.423(9) . ?
C19 C20 1.404(9) . ?
C20 C401 1.506(9) . ?
C101 C106 1.382(12) . ?
C101 C102 1.384(11) . ?
C102 C103 1.364(13) . ?
C103 C104 1.344(18) . ?
C104 C105 1.38(2) . ?
C105 C106 1.367(14) . ?
C111 O11 1.109(9) . ?
C112 O12 1.129(9) . ?
C113 O13 1.132(9) . ?
C201 C202 1.369(10) . ?
C201 C206 1.378(11) . ?
C202 C203 1.390(11) . ?
C203 C204 1.321(15) . ?
C204 C205 1.372(15) . ?
C205 C206 1.406(12) . ?
C221 O21 1.121(9) . ?
C222 O22 1.145(9) . ?
C223 O23 1.138(9) . ?
C301 C302 1.366(14) . ?
C301 C306 1.392(13) . ?
C302 C303 1.380(14) . ?
C303 C304 1.34(2) . ?
C304 C305 1.34(2) . ?
C305 C306 1.418(15) . ?
C331 O31 1.128(10) . ?
C332 O32 1.136(9) . ?
C333 O33 1.130(8) . ?
C401 C406 1.341(12) . ?
C401 C402 1.379(11) . ?
C402 C403 1.373(13) . ?
C403 C404 1.347(16) . ?
C404 C405 1.329(16) . ?
C405 C406 1.394(13) . ?
N5 C505 1.377(10) . ?
C505 C504 1.374(12) . ?
C502 C503 1.369(14) . ?
C504 C503 1.345(15) . ?
C602 C601 1.266(16) . ?
C602 C603 1.288(16) . ?
C602 C604 1.92(4) . ?
C602 C606 2.01(4) . ?
C603 C604 1.267(16) . ?
C604 C605 1.283(17) . ?
C605 C606 1.289(17) . ?
C601 C606 1.273(17) . ?
C601 C607 1.38(4) . ?
C606 C607 2.03(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C112 Os1 C113 92.3(4) . . ?
C112 Os1 C111 90.4(4) . . ?
C113 Os1 C111 168.1(3) . . ?
C112 Os1 In 86.5(2) . . ?
C113 Os1 In 83.2(2) . . ?
C111 Os1 In 85.4(2) . . ?
C112 Os1 Os2 164.4(2) . . ?
C113 Os1 Os2 91.3(2) . . ?
C111 Os1 Os2 89.2(2) . . ?
In Os1 Os2 108.98(3) . . ?
C112 Os1 Os3 110.4(2) . . ?
C113 Os1 Os3 96.7(2) . . ?
C111 Os1 Os3 93.3(2) . . ?
In Os1 Os3 163.026(16) . . ?
Os2 Os1 Os3 54.06(2) . . ?
C222 Os2 C223 94.5(3) . . ?
C222 Os2 C221 94.0(3) . . ?
C223 Os2 C221 91.2(3) . . ?
C222 Os2 N5 95.5(3) . . ?
C223 Os2 N5 89.1(3) . . ?
C221 Os2 N5 170.5(3) . . ?
C222 Os2 Os3 165.3(2) . . ?
C223 Os2 Os3 87.0(2) . . ?
C221 Os2 Os3 100.6(2) . . ?
N5 Os2 Os3 69.89(18) . . ?
C222 Os2 Os1 114.8(2) . . ?
C223 Os2 Os1 150.3(2) . . ?
C221 Os2 Os1 91.5(2) . . ?
N5 Os2 Os1 83.61(16) . . ?
Os3 Os2 Os1 63.43(3) . . ?
C333 Os3 C332 94.8(3) . . ?
C333 Os3 C331 91.4(3) . . ?
C332 Os3 C331 98.5(4) . . ?
C333 Os3 C501 89.1(3) . . ?
C332 Os3 C501 98.3(4) . . ?
C331 Os3 C501 163.0(3) . . ?
C333 Os3 Os2 97.5(2) . . ?
C332 Os3 Os2 163.3(3) . . ?
C331 Os3 Os2 92.3(3) . . ?
C501 Os3 Os2 70.81(17) . . ?
C333 Os3 Os1 160.0(2) . . ?
C332 Os3 Os1 104.6(2) . . ?
C331 Os3 Os1 90.3(2) . . ?
C501 Os3 Os1 83.66(16) . . ?
Os2 Os3 Os1 62.510(19) . . ?
N2 In N3 83.03(19) . . ?
N2 In N4 136.7(2) . . ?
N3 In N4 82.72(19) . . ?
N2 In N1 82.28(19) . . ?
N3 In N1 138.5(2) . . ?
N4 In N1 81.95(19) . . ?
N2 In Os1 114.14(13) . . ?
N3 In Os1 109.93(15) . . ?
N4 In Os1 109.12(15) . . ?
N1 In Os1 111.52(14) . . ?
C4 N1 C1 106.8(5) . . ?
C4 N1 In 124.2(4) . . ?
C1 N1 In 123.1(4) . . ?
C6 N2 C9 106.8(5) . . ?
C6 N2 In 124.8(4) . . ?
C9 N2 In 126.0(4) . . ?
C11 N3 C14 107.9(5) . . ?
C11 N3 In 124.6(4) . . ?
C14 N3 In 124.4(4) . . ?
C19 N4 C16 107.0(5) . . ?
C19 N4 In 124.6(4) . . ?
C16 N4 In 123.9(4) . . ?
C502 C501 N5 119.7(7) . . ?
C502 C501 Os3 131.8(6) . . ?
N5 C501 Os3 108.4(4) . . ?
N1 C1 C20 125.2(6) . . ?
N1 C1 C2 109.8(6) . . ?
C20 C1 C2 125.0(6) . . ?
C3 C2 C1 106.8(6) . . ?
C2 C3 C4 107.9(6) . . ?
N1 C4 C5 124.8(5) . . ?
N1 C4 C3 108.7(5) . . ?
C5 C4 C3 126.5(6) . . ?
C6 C5 C4 126.2(6) . . ?
C6 C5 C101 117.5(6) . . ?
C4 C5 C101 116.4(6) . . ?
N2 C6 C5 126.0(6) . . ?
N2 C6 C7 108.5(5) . . ?
C5 C6 C7 125.4(6) . . ?
C8 C7 C6 108.0(6) . . ?
C7 C8 C9 107.3(6) . . ?
N2 C9 C10 125.4(6) . . ?
N2 C9 C8 109.5(5) . . ?
C10 C9 C8 125.1(6) . . ?
C11 C10 C9 125.5(6) . . ?
C11 C10 C201 118.0(6) . . ?
C9 C10 C201 116.4(6) . . ?
N3 C11 C10 126.2(6) . . ?
N3 C11 C12 108.4(6) . . ?
C10 C11 C12 125.2(6) . . ?
C13 C12 C11 107.0(6) . . ?
C12 C13 C14 108.4(6) . . ?
N3 C14 C15 125.6(6) . . ?
N3 C14 C13 108.3(6) . . ?
C15 C14 C13 126.1(6) . . ?
C16 C15 C14 125.5(6) . . ?
C16 C15 C301 117.4(6) . . ?
C14 C15 C301 117.1(6) . . ?
N4 C16 C15 126.6(6) . . ?
N4 C16 C17 107.9(6) . . ?
C15 C16 C17 125.5(6) . . ?
C18 C17 C16 107.8(7) . . ?
C17 C18 C19 108.1(6) . . ?
N4 C19 C20 125.4(6) . . ?
N4 C19 C18 109.2(6) . . ?
C20 C19 C18 125.4(6) . . ?
C1 C20 C19 125.9(6) . . ?
C1 C20 C401 116.9(6) . . ?
C19 C20 C401 117.1(6) . . ?
C106 C101 C102 116.8(8) . . ?
C106 C101 C5 120.8(7) . . ?
C102 C101 C5 122.4(7) . . ?
C103 C102 C101 120.8(10) . . ?
C104 C103 C102 121.2(11) . . ?
C103 C104 C105 119.9(10) . . ?
C106 C105 C104 118.8(12) . . ?
C105 C106 C101 122.4(11) . . ?
O11 C111 Os1 177.8(7) . . ?
O12 C112 Os1 178.9(9) . . ?
O13 C113 Os1 176.5(7) . . ?
C202 C201 C206 118.1(7) . . ?
C202 C201 C10 122.3(7) . . ?
C206 C201 C10 119.6(7) . . ?
C201 C202 C203 120.4(9) . . ?
C204 C203 C202 122.3(9) . . ?
C203 C204 C205 118.9(8) . . ?
C204 C205 C206 120.2(10) . . ?
C201 C206 C205 120.1(9) . . ?
O21 C221 Os2 179.6(8) . . ?
O22 C222 Os2 175.0(7) . . ?
O23 C223 Os2 178.1(7) . . ?
C302 C301 C306 119.7(9) . . ?
C302 C301 C15 119.5(8) . . ?
C306 C301 C15 120.8(9) . . ?
C301 C302 C303 121.0(12) . . ?
C304 C303 C302 120.7(14) . . ?
C303 C304 C305 119.2(11) . . ?
C304 C305 C306 122.8(13) . . ?
C301 C306 C305 116.5(12) . . ?
O31 C331 Os3 175.9(8) . . ?
O32 C332 Os3 177.7(8) . . ?
O33 C333 Os3 178.7(8) . . ?
C406 C401 C402 117.3(7) . . ?
C406 C401 C20 121.3(7) . . ?
C402 C401 C20 121.4(7) . . ?
C403 C402 C401 121.3(10) . . ?
C404 C403 C402 119.8(11) . . ?
C405 C404 C403 120.1(9) . . ?
C404 C405 C406 120.2(11) . . ?
C401 C406 C405 121.2(10) . . ?
C501 N5 C505 119.6(6) . . ?
C501 N5 Os2 110.9(5) . . ?
C505 N5 Os2 129.5(5) . . ?
C504 C505 N5 120.0(8) . . ?
C501 C502 C503 121.2(9) . . ?
C503 C504 C505 119.8(9) . . ?
C504 C503 C502 119.6(9) . . ?
C601 C602 C603 149(3) . . ?
C601 C602 C604 108(2) . . ?
C603 C602 C604 40.9(13) . . ?
C601 C602 C606 37.7(15) . . ?
C603 C602 C606 111(2) . . ?
C604 C602 C606 70.0(12) . . ?
C604 C603 C602 97(2) . . ?
C603 C604 C605 127(3) . . ?
C603 C604 C602 41.7(13) . . ?
C605 C604 C602 86(2) . . ?
C604 C605 C606 123(3) . . ?
C602 C601 C606 105(3) . . ?
C602 C601 C607 155(3) . . ?
C606 C601 C607 100(3) . . ?
C601 C606 C605 119(3) . . ?
C601 C606 C602 37.5(15) . . ?
C605 C606 C602 82(2) . . ?
C601 C606 C607 42.2(17) . . ?
C605 C606 C607 161(3) . . ?
C602 C606 C607 79.5(17) . . ?
C601 C607 C606 38.1(14) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.151
_refine_diff_density_min         -1.869
_refine_diff_density_rms         0.155