Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Wagner Matthias' 'Jan W. Bats' 'Michael Bolte' 'Hans-Wolfram Lerner' 'Gunter Margraf' _publ_contact_author_name 'Prof Matthias Wagner' _publ_contact_author_address ; Institut fuer Anorganische Chemie Goethe-Universitaet Frankfurt Marie Curie-Strasse 11 Frankfurt 60439 GERMANY ; _publ_contact_author_email 'MATTHIAS.WAGNER@CHEMIE.UNI-FRANKFURT.DE' _publ_requested_journal 'Chemical Communications' _publ_section_title ; One- and three-dimensional infinite arrays of Cu(I) centres exhibited by [Cu(NH3)2]Br and [Cu(NH3)Cl] in the solid state. ; data_margraf2 _database_code_CSD 200580 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H3 Cl Cu N' _chemical_formula_weight 116.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'N' 'N' 0.0061 0.0033 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'I 213' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 8.4135(8) _cell_length_b 8.4135(8) _cell_length_c 8.4135(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 595.57(10) _cell_formula_units_Z 8 _cell_measurement_temperature 146(2) _cell_measurement_reflns_used 188 _cell_measurement_theta_min 3 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 7.898 _exptl_absorpt_correction_type 'numerical (SHELXTL, Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.334 _exptl_absorpt_correction_T_max 0.424 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 146(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type SIEMENS_SMART_CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 131 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 600 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 6829 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 37.10 _reflns_number_total 505 _reflns_number_gt 485 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'H atom parameters refined' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0172(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(2) _refine_ls_number_reflns 505 _refine_ls_number_parameters 16 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0217 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0420 _refine_ls_wR_factor_gt 0.0411 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.000 _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 Cu Cu -0.11817(3) -0.11817(3) -0.11817(3) 0.01736(10) Uani 1 3 d S . . N N 0.01181(17) 0.01181(17) 0.01181(17) 0.0211(4) Uani 1 3 d S . . Cl Cl -0.26265(4) -0.26265(4) -0.26265(4) 0.02018(13) Uani 1 3 d S . . H H 0.075(4) -0.035(5) 0.082(4) 0.036(9) Uiso 1 1 d . . . 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 Cu 0.01736(10) 0.01736(10) 0.01736(10) -0.00241(7) -0.00241(7) -0.00241(7) N 0.0211(4) 0.0211(4) 0.0211(4) -0.0033(5) -0.0033(5) -0.0033(5) Cl 0.02018(13) 0.02018(13) 0.02018(13) -0.00347(13) -0.00347(13) -0.00347(13) _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 Cu N 1.894(3) . ? Cu Cl 2.1054(8) . ? Cu Cu 2.9791(3) 16_444 ? Cu Cu 2.9791(3) 14_444 ? Cu Cu 2.9791(3) 15_444 ? N H 0.88(3) . ? 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 N Cu Cl 180.00(11) . . ? N Cu Cu 92.552(10) . 16_444 ? Cl Cu Cu 87.448(10) . 16_444 ? N Cu Cu 92.552(10) . 14_444 ? Cl Cu Cu 87.448(10) . 14_444 ? Cu Cu Cu 119.804(2) 16_444 14_444 ? N Cu Cu 92.552(10) . 15_444 ? Cl Cu Cu 87.448(10) . 15_444 ? Cu Cu Cu 119.804(2) 16_444 15_444 ? Cu Cu Cu 119.803(2) 14_444 15_444 ? Cu N H 118(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N H Cl 0.89(4) 2.66(4) 3.528(2) 167(3) 4_545 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 37.10 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.458 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.090 #===END data_wa116 _database_code_CSD 200581 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H6 Br Cu N2' _chemical_formula_weight 177.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 6.6020(10) _cell_length_b 12.879(2) _cell_length_c 5.8610(10) _cell_angle_alpha 90.00 _cell_angle_beta 114.91(2) _cell_angle_gamma 90.00 _cell_volume 451.98(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6744 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 29.7 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 13.472 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.1337 _exptl_absorpt_correction_T_max 0.5523 _exptl_absorpt_process_details 'MULABS (Spek, 1990; Blessing, 1995)' _exptl_special_details ; ; ; _diffrn_ambient_temperature 100(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4925 _diffrn_reflns_av_R_equivalents 0.1280 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 29.64 _reflns_number_total 641 _reflns_number_gt 558 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material ? _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^)+(0.0364P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0122(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 641 _refine_ls_number_parameters 34 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0708 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _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 Br1 Br 0.5000 0.13244(3) 0.2500 0.02117(18) Uani 1 2 d S . . Cu1 Cu 0.5000 0.5000 0.0000 0.02129(19) Uani 1 2 d S . . N1 N 0.6777(6) 0.3781(2) 0.0977(6) 0.0227(5) Uani 1 1 d . . . H2 H 0.799(12) 0.378(4) 0.274(12) 0.055(19) Uiso 1 1 d . . . H3 H 0.764(15) 0.371(5) 0.009(14) 0.06(2) Uiso 1 1 d . . . H1 H 0.619(9) 0.324(5) 0.088(9) 0.031(12) Uiso 1 1 d . . . 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 Br1 0.0237(3) 0.0224(3) 0.0194(2) 0.000 0.01108(17) 0.000 Cu1 0.0248(3) 0.0214(3) 0.0196(3) 0.00237(16) 0.0113(2) 0.00459(17) N1 0.0244(13) 0.0227(14) 0.0233(13) 0.0015(9) 0.0121(11) 0.0029(10) _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 Cu1 N1 1.898(3) 5_665 ? Cu1 N1 1.898(3) . ? Cu1 Cu1 2.9305(5) 2_654 ? Cu1 Cu1 2.9305(5) 2_655 ? N1 H2 1.01(7) . ? N1 H3 0.92(8) . ? N1 H1 0.78(6) . ? 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 N1 Cu1 N1 180.00(10) 5_665 . ? N1 Cu1 Cu1 87.63(9) 5_665 2_654 ? N1 Cu1 Cu1 92.37(9) . 2_654 ? N1 Cu1 Cu1 92.37(9) 5_665 2_655 ? N1 Cu1 Cu1 87.63(9) . 2_655 ? Cu1 Cu1 Cu1 180.0 2_654 2_655 ? Cu1 N1 H2 116(3) . . ? Cu1 N1 H3 111(4) . . ? H2 N1 H3 99(7) . . ? Cu1 N1 H1 119(4) . . ? H2 N1 H1 103(5) . . ? H3 N1 H1 106(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Br1 0.78(6) 2.87(6) 3.614(3) 159(4) . N1 H3 Br1 0.92(8) 2.59(8) 3.515(3) 175(6) 7_655 N1 H2 Br1 1.01(7) 2.54(7) 3.508(3) 162(5) 7_656 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.64 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.015 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.175