# Supplementary Material (ESI) for Chemical Communications

# This journal is © The Royal Society of Chemistry 2002



data_global

_audit_creation_date            02-07-25

_audit_creation_method          CRYSTALS

_publ_contact_letter

;

 These are the CIF format data (1 compound) for the paper 



  "Synthesis and reactivity of the imidotungsten methyl cation

  [W(N2Npy)(NPh)Me]+: CO2 adds to the W=NPh bond and does not insert 

  into the W-Me bond"



B D Ward, E Clot, S Dubberley, L H Gade and P. Mountford





;

_publ_contact_author

;

 Dr P. Mountford           

 Inorganic Chemistry Laboratory

 South Parks Road

 Oxford

 OX1 3QR

 UK

;                                           

_publ_contact_author_phone      '+44 1865 272679

_contact_author_fax             '+44 1865 272690'

_publ_contact_author_email      Philip.Mountford@chem.ox.ac.uk





data_COMPOUND_2



#  Local code BDW5 

                                                                                

                                                                                

_chemical_name_systematic                                                       

;                                                                               

 [W{(2-C5NH4)C(Me)(CH2NSiMe3)2}(NPh)Me2]                                                                              

;                                                                               

_publ_section_exptl_refinement                                                  

;                                                                               

 No special details                                                                              

;                                                                               

_cell_length_a    			10.6452(2)       

_cell_length_b    			16.4633(3)       

_cell_length_c    			15.2794(2)       

_cell_angle_alpha    			90.00            

_cell_angle_beta      			91.659(1)       

_cell_angle_gamma    			90.00            

_cell_volume      			2676.67(8)       

_symmetry_cell_setting 			'Monoclinic ' 

_symmetry_space_group_name_H-M 	'P 1 21/n 1 ' 

loop_

 _symmetry_equiv_pos_as_xyz

 'x,y,z'

 '-x,-y,-z'

 '-x+1/2,y+1/2,-z+1/2'

 'x+1/2,-y+1/2,z+1/2'

loop_

_atom_type_symbol

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_Cromer_Mann_a1

_atom_type_scat_Cromer_Mann_b1

_atom_type_scat_Cromer_Mann_a2

_atom_type_scat_Cromer_Mann_b2

_atom_type_scat_Cromer_Mann_a3

_atom_type_scat_Cromer_Mann_b3

_atom_type_scat_Cromer_Mann_a4

_atom_type_scat_Cromer_Mann_b4

_atom_type_scat_Cromer_Mann_c

_atom_type_scat_source  

 'C   '    0.0020    0.0020    2.3100   20.8439

    1.0200   10.2075    1.5886    0.5687    0.8650   51.6512    0.2156

'International_Tables_Vol_IV_Table_2.2B'

 'H   '    0.0000    0.0000    0.4930   10.5109

    0.3229   26.1257    0.1402    3.1424    0.0408   57.7997    0.0030

'International_Tables_Vol_IV_Table_2.2B'

 'N   '    0.0040    0.0030   12.2126    0.0057

    3.1322    9.8933    2.0125   28.9975    1.1663    0.5826  -11.5290

'International_Tables_Vol_IV_Table_2.2B'

 'W   '   -1.4210    6.8720   29.0818    1.7203

   15.4300    9.2259   14.4327    0.3217    5.1198   57.0560    9.8875

'International_Tables_Vol_IV_Table_2.2B'

 'Si  '    0.0720    0.0710    6.2915    2.4386

    3.0353   32.3337    1.9891    0.6785    1.5410   81.6937    1.1407

'International_Tables_Vol_IV_Table_2.2B'

_chemical_formula_sum

' C23 H40 N4 Si2 W1 '

_chemical_formula_moiety

' C23 H40 N4 Si2 W1 '

_chemical_compound_source

;

?

;

_chemical_formula_weight   			612.62

_cell_measurement_temperature    		150

_cell_measurement_reflns_used     		6261

_cell_measurement_theta_min        		2.910

_cell_measurement_theta_max        		27.485

_cell_formula_units_Z 				4		

_exptl_crystal_description 			'block ' 

_exptl_crystal_colour 				'dark red' 

_exptl_crystal_size_min 			0.10 

_exptl_crystal_size_mid 			0.20 

_exptl_crystal_size_max 			0.30 

_exptl_crystal_density_diffrn 		1.52 

_exptl_crystal_density_method           	none                

_exptl_crystal_density_meas 			'not measured' 

_exptl_crystal_F_000 				1227.09

_exptl_absorpt_coefficient_mu 		4.42 

_exptl_absorpt_correction_type          	'multi-scan'       

_exptl_absorpt_correction_T_min         	0.413               

_exptl_absorpt_correction_T_max         	0.643                  

_diffrn_ambient_temperature        		150

_diffrn_standards_interval_time         'not measured'                          

_diffrn_standards_interval_count        'not measured'                          

_diffrn_standards_number                'not measured'                          

_diffrn_standards_decay_%               'not measured'                          

_diffrn_measurement_device_type         'Nonius KappaCCD'                       

_diffrn_radiation_type       			'Mo K\a'

_diffrn_radiation_wavelength      		0.71073

_diffrn_measurement_method 			'CCD'

_diffrn_reflns_number 				12044 

_reflns_number_total 				6111 

_diffrn_reflns_av_R_equivalents 		0.01 

_reflns_number_gt 				4338 

_diffrn_reflns_theta_min 			2.91 

_diffrn_reflns_theta_max  			27.47

_diffrn_reflns_limit_h_min 			-13 

_diffrn_reflns_limit_h_max 			13 

_diffrn_reflns_limit_k_min 			-21 

_diffrn_reflns_limit_k_max 			21 

_diffrn_reflns_limit_l_min 			-19 

_diffrn_reflns_limit_l_max			 19 

_reflns_limit_h_min 				-13 

_reflns_limit_h_max 				13 

_reflns_limit_k_min 				0 

_reflns_limit_k_max 				21 

_reflns_limit_l_min 				0 

_reflns_limit_l_max 				19 

_refine_diff_density_min 			-0.60 

_refine_diff_density_max 			1.19 

_reflns_threshold_expression  		>3.00σ(I)

_refine_ls_number_reflns 			4338 

_refine_ls_number_parameters 			272 

_refine_ls_R_factor_gt 				0.0227 

_refine_ls_wR_factor_ref 			0.0106 

_refine_ls_goodness_of_fit_ref 		1.2430 

_refine_ls_shift/su_max 			0.01 

_refine_ls_structure_factor_coef 		F 

_refine_ls_weighting_scheme             'Chebychev polynomial'                  

_refine_ls_weighting_details 

;

Chebychev polynomial with 2 parameters, Carruthers & Watkin , 1979, 

0.828E-01-.519    

;

_refine_ls_hydrogen_treatment           'riding model'                          

_atom_sites_solution_primary            'direct methods'                        

_atom_sites_solution_hydrogens          geometric                               

_refine_ls_matrix_type                  full                                    

_refine_ls_number_restraints            0

_refine_ls_abs_structure_flack          none

_refine_ls_extinction_coef 			71.1(39) 

_refine_ls_extinction_method 

    'Larson 1970 Crystallographic Computing eq 22'



_computing_data_collection                                                      

;                                                                               

KappaCCD software 'Collect' (Nonius, 2000)                                      

;                                                                               

_computing_data_reduction                                                       

;                                                                               

KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)                            

;                                                                               

_computing_cell_refinement                                                      

;                                                                               

KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)                            

;                                                                               

_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'               

_computing_structure_refinement                                                 

;                                                                               

CRYSTALS Issue 10 (Watkin et al., 1996)                                         

;                                                                               

_computing_molecular_graphics  'CAMERON (Watkin, Prout and Pearce, 1996)'       

                                                                                

_computing_publication_material                                                 

;                                                                               

CRYSTALS Issue 10 (Watkin et al., 1996)                                         

;                                                                               



loop_

_atom_site_label

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_occupancy

_atom_site_adp_type

W1 0.237863(6) 0.247246(7) 0.386340(4) 0.0172 1.0000 Uani 

N1 0.10629(18) 0.30981(11) 0.39420(12) 0.0216 1.0000 Uani 

N2 0.22724(17) 0.1635(1) 0.48039(11) 0.0207 1.0000 Uani 

N3 0.19528(16) 0.15889(11) 0.2965(1) 0.0201 1.0000 Uani 

N4 0.43910(17) 0.19381(11) 0.37012(11) 0.0222 1.0000 Uani 

Si1 0.11065(6) 0.16617(4) 0.56007(4) 0.0261 1.0000 Uani 

Si2 0.10304(5) 0.16757(4) 0.20055(4) 0.0227 1.0000 Uani 

C1 0.0234(2) 0.37564(12) 0.39351(13) 0.0197 1.0000 Uani 

C2 0.0675(2) 0.45246(14) 0.37170(16) 0.0290 1.0000 Uani 

C3 -0.0154(3) 0.51753(15) 0.36860(17) 0.0368 1.0000 Uani 

C4 -0.1399(3) 0.50687(15) 0.38618(18) 0.0356 1.0000 Uani 

C5 -0.1836(2) 0.43054(16) 0.40947(18) 0.0346 1.0000 Uani 

C6 -0.1028(2) 0.36493(15) 0.41378(15) 0.0290 1.0000 Uani 

C7 0.3051(2) 0.32113(13) 0.27299(13) 0.0269 1.0000 Uani 

C8 0.3512(2) 0.32977(14) 0.47298(14) 0.0273 1.0000 Uani 

C9 0.53839(19) 0.2426(2) 0.35656(12) 0.0285 1.0000 Uani 

C10 0.6569(2) 0.21364(17) 0.33946(16) 0.0336 1.0000 Uani 

C11 0.6748(2) 0.13045(19) 0.33521(18) 0.0391 1.0000 Uani 

C12 0.5740(2) 0.07971(17) 0.35014(15) 0.0307 1.0000 Uani 

C13 0.4563(2) 0.11259(13) 0.36734(14) 0.0225 1.0000 Uani 

C14 0.3419(2) 0.06276(14) 0.38534(14) 0.0252 1.0000 Uani 

C15 0.3715(2) -0.02865(14) 0.38796(17) 0.0310 1.0000 Uani 

C16 0.2926(2) 0.08577(13) 0.47581(15) 0.0248 1.0000 Uani 

C17 0.2401(2) 0.07519(12) 0.31209(15) 0.0264 1.0000 Uani 

C18 -0.0387(3) 0.12820(18) 0.5087(2) 0.0512 1.0000 Uani 

C19 0.0881(2) 0.26955(13) 0.60582(15) 0.0309 1.0000 Uani 

C20 0.1575(3) 0.09837(17) 0.65424(19) 0.0498 1.0000 Uani 

C21 0.0135(3) 0.07131(16) 0.18181(18) 0.0399 1.0000 Uani 

C22 -0.01582(17) 0.2509(2) 0.20680(13) 0.0302 1.0000 Uani 

C23 0.2017(2) 0.18346(19) 0.10303(15) 0.0383 1.0000 Uani 

H21 0.1582 0.46038 0.35847 0.0360 1.0000 Uiso 

H31 0.0163 0.57277 0.35333 0.0442 1.0000 Uiso 

H41 -0.1992 0.55392 0.38250 0.0433 1.0000 Uiso 

H51 -0.2743 0.42279 0.42274 0.0410 1.0000 Uiso 

H61 -0.1339 0.31020 0.43150 0.0358 1.0000 Uiso 

H71 0.3860 0.29812 0.25228 0.0351 1.0000 Uiso 

H72 0.3188 0.37871 0.29208 0.0351 1.0000 Uiso 

H73 0.2406 0.31964 0.22411 0.0351 1.0000 Uiso 

H81 0.4380 0.30757 0.48086 0.0354 1.0000 Uiso 

H82 0.3110 0.33390 0.53118 0.0354 1.0000 Uiso 

H83 0.3548 0.38488 0.44561 0.0354 1.0000 Uiso 

H91 0.52550 0.3027 0.35899 0.0351 1.0000 Uiso 

H101 0.7286 0.25165 0.33032 0.0433 1.0000 Uiso 

H111 0.7589 0.10737 0.32158 0.0461 1.0000 Uiso 

H121 0.5851 0.01941 0.34874 0.0375 1.0000 Uiso 

H151 0.2930 -0.05954 0.40021 0.0395 1.0000 Uiso 

H152 0.4362 -0.03974 0.43521 0.0395 1.0000 Uiso 

H153 0.4043 -0.04614 0.33025 0.0395 1.0000 Uiso 

H161 0.3661 0.08748 0.51811 0.0315 1.0000 Uiso 

H162 0.2330 0.04232 0.49377 0.0315 1.0000 Uiso 

H171 0.1656 0.04149 0.32722 0.0338 1.0000 Uiso 

H172 0.2755 0.05497 0.25623 0.0338 1.0000 Uiso 

H181 -0.1069 0.12886 0.5523 0.0621 1.0000 Uiso 

H182 -0.0261 0.07141 0.4875 0.0621 1.0000 Uiso 

H183 -0.0628 0.16398 0.4581 0.0621 1.0000 Uiso 

H191 0.0213 0.26798 0.65049 0.0391 1.0000 Uiso 

H192 0.1688 0.28862 0.63397 0.0391 1.0000 Uiso 

H193 0.0623 0.30770 0.55764 0.0391 1.0000 Uiso 

H201 0.0914 0.09979 0.69937 0.0624 1.0000 Uiso 

H202 0.2390 0.11798 0.68071 0.0624 1.0000 Uiso 

H203 0.1678 0.04143 0.63281 0.0624 1.0000 Uiso 

H211 -0.0395 0.07617 0.12696 0.0498 1.0000 Uiso 

H212 -0.0416 0.06100 0.23253 0.0498 1.0000 Uiso 

H213 0.0738 0.02518 0.17591 0.0498 1.0000 Uiso 

H221 -0.06626 0.2536 0.15063 0.0383 1.0000 Uiso 

H222 0.02826 0.3039 0.21699 0.0383 1.0000 Uiso 

H223 -0.07292 0.2399 0.25625 0.0383 1.0000 Uiso 

H231 0.1464 0.18826 0.04929 0.0490 1.0000 Uiso 

H232 0.2518 0.23447 0.11104 0.0490 1.0000 Uiso 

H233 0.2601 0.13635 0.09659 0.0490 1.0000 Uiso 


loop_

 _geom_bond_atom_site_label_1

 _geom_bond_site_symmetry_1

 _geom_bond_atom_site_label_2

 _geom_bond_site_symmetry_2

 _geom_bond_distance

 _geom_bond_publ_flag

W1 . N1 . 1.7455(18)    yes

W1 . N2 . 1.9968(17)    yes

W1 . N3 . 2.0416(17)    yes

W1 . N4 . 2.3357(18)    yes

W1 . C7 . 2.250(2)    yes

W1 . C8 . 2.228(2)    yes

N1 . C1 . 1.397(3)    yes

N2 . Si1 . 1.7641(18)    yes

N2 . C16 . 1.460(3)    yes

N3 . Si2 . 1.7471(17)    yes

N3 . C17 . 1.475(3)    yes

N4 . C9 . 1.348(3)    yes

N4 . C13 . 1.350(3)    yes

Si1 . C18 . 1.860(3)    yes

Si1 . C19 . 1.858(2)    yes

Si1 . C20 . 1.877(3)    yes

Si2 . C21 . 1.867(3)    yes

Si2 . C22 . 1.871(3)    yes

Si2 . C23 . 1.866(3)    yes

C1 . C2 . 1.393(3)    yes

C1 . C6 . 1.399(3)    yes

C2 . C3 . 1.388(3)    yes

C3 . C4 . 1.371(4)    yes

C4 . C5 . 1.390(4)    yes

C5 . C6 . 1.382(3)    yes

C9 . C10 . 1.380(3)    yes

C10 . C11 . 1.385(4)    yes

C11 . C12 . 1.384(4)    yes

C12 . C13 . 1.397(3)    yes

C13 . C14 . 1.500(3)    yes

C14 . C15 . 1.538(3)    yes

C14 . C16 . 1.540(3)    yes

C14 . C17 . 1.549(3)    yes

loop_

 _geom_angle_atom_site_label_1

 _geom_angle_site_symmetry_1

 _geom_angle_atom_site_label_2

 _geom_angle_site_symmetry_2

 _geom_angle_atom_site_label_3

 _geom_angle_site_symmetry_3

 _geom_angle

 _geom_angle_publ_flag

N1 . W1 . N2 . 107.19(8)    yes

N1 . W1 . N3 . 107.68(8)    yes

N2 . W1 . N3 . 88.61(7)    yes

N1 . W1 . N4 . 165.89(7)    yes

N2 . W1 . N4 . 83.55(7)    yes

N3 . W1 . N4 . 81.19(7)    yes

N1 . W1 . C7 . 90.45(8)    yes

N2 . W1 . C7 . 162.36(8)    yes

N3 . W1 . C7 . 86.40(7)    yes

N4 . W1 . C7 . 78.97(7)    yes

N1 . W1 . C8 . 91.21(9)    yes

N2 . W1 . C8 . 91.97(8)    yes

N3 . W1 . C8 . 160.03(8)    yes

N4 . W1 . C8 . 79.05(8)    yes

C7 . W1 . C8 . 87.06(8)    yes

W1 . N1 . C1 . 164.76(16)    yes

W1 . N2 . Si1 . 122.36(9)    yes

W1 . N2 . C16 . 122.26(14)    yes

Si1 . N2 . C16 . 113.63(14)    yes

W1 . N3 . Si2 . 127.9(1)    yes

W1 . N3 . C17 . 119.53(13)    yes

Si2 . N3 . C17 . 112.51(13)    yes

W1 . N4 . C9 . 121.17(17)    yes

W1 . N4 . C13 . 120.13(15)    yes

C9 . N4 . C13 . 118.5(2)    yes

N2 . Si1 . C18 . 108.08(12)    yes

N2 . Si1 . C19 . 112.5(1)    yes

C18 . Si1 . C19 . 110.39(12)    yes

N2 . Si1 . C20 . 109.72(11)    yes

C18 . Si1 . C20 . 109.17(16)    yes

C19 . Si1 . C20 . 106.90(13)    yes

N3 . Si2 . C21 . 109.4(1)    yes

N3 . Si2 . C22 . 112.43(9)    yes

C21 . Si2 . C22 . 106.69(12)    yes

N3 . Si2 . C23 . 111.5(1)    yes

C21 . Si2 . C23 . 107.06(13)    yes

C22 . Si2 . C23 . 109.58(12)    yes

N1 . C1 . C2 . 119.29(18)    yes

N1 . C1 . C6 . 120.7(2)    yes

C2 . C1 . C6 . 120.0(2)    yes

C1 . C2 . C3 . 119.4(2)    yes

C2 . C3 . C4 . 120.8(2)    yes

C3 . C4 . C5 . 119.9(2)    yes

C4 . C5 . C6 . 120.4(2)    yes

C1 . C6 . C5 . 119.5(2)    yes

N4 . C9 . C10 . 123.3(3)    yes

C9 . C10 . C11 . 118.6(3)    yes

C10 . C11 . C12 . 118.7(2)    yes

C11 . C12 . C13 . 120.1(2)    yes

N4 . C13 . C12 . 120.8(2)    yes

N4 . C13 . C14 . 115.09(18)    yes

C12 . C13 . C14 . 124.1(2)    yes

C13 . C14 . C15 . 111.91(18)    yes

C13 . C14 . C16 . 109.23(18)    yes

C15 . C14 . C16 . 106.99(18)    yes

C13 . C14 . C17 . 110.49(18)    yes

C15 . C14 . C17 . 106.66(18)    yes

C16 . C14 . C17 . 111.52(17)    yes

N2 . C16 . C14 . 115.72(18)    yes

N3 . C17 . C14 . 117.14(17)    yes

