Unique Approach to Copper(I) Silylene Chalcogenone Complexes.
Parvin, Nasrina; Pal, Shiv; Khan, Shabana; Das, Shubhajit; Pati, Swapan K.; Roesky, Herbert W.; Inorganic chemistry 56 (2017) 1706–1712; doi:10.1021/acs.inorgchem.6b02833

data_4345443
_publ_section_title
;
 Unique Approach to Copper(I) Silylene Chalcogenone Complexes.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1706
_journal_page_last               1712
_journal_paper_doi               10.1021/acs.inorgchem.6b02833
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C69 H56 Br Cu N2 Se, C7H8'
_chemical_formula_sum            'C76 H64 Br Cu N2 Se'
_chemical_formula_weight         1227.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.715(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.191(12)
_cell_length_b                   12.807(7)
_cell_length_c                   25.044(14)
_cell_measurement_reflns_used    9367
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.45
_cell_measurement_theta_min      2.29
_cell_volume                     6699(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2240
_diffrn_reflns_av_unetI/netI     0.1481
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            92225
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        22.499
_diffrn_reflns_theta_max         22.499
_diffrn_reflns_theta_min         2.332
_exptl_absorpt_coefficient_mu    1.507
_exptl_absorpt_process_details
'Sheldrick, G. M. (2012) SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       block
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.6039
_platon_squeeze_details
;
TITL 14_a.res in P2(1)/c
CELL   21.1910   12.8070   25.0440     90.00     99.71     90.00
SPGR P21/c
C101 0.541 0.174 0.056 !       3.29 eA-3
C102 0.618 0.147 0.073 !       2.67 eA-3
C103 0.490 0.215 0.071 !       2.48 eA-3
C104 0.479 0.662 0.391 !       2.45 eA-3
C105 0.555 0.076 0.003 !       2.35 eA-3
C106 0.518 0.162 0.017 !       2.32 eA-3
C107 0.409 0.683 0.468 !       2.31 eA-3
C108 0.610 0.364 0.462 !       2.28 eA-3
C109 0.595 0.392 0.451 !       2.27 eA-3
C110 0.402 0.780 0.023 !       2.21 eA-3
C111 0.554 0.173 0.010 !       2.20 eA-3
C112 0.622 0.206 0.000 !       2.14 eA-3
C113 0.453 0.703 0.406 !       2.05 eA-3
C114 0.428 0.753 0.469 !       2.02 eA-3
C115 0.493 0.722 0.398 !       1.98 eA-3
C116 0.416 0.738 0.009 !       1.94 eA-3
C117 0.569 0.312 0.436 !       1.93 eA-3
C118 0.488 0.829 0.022 !       1.88 eA-3
C119 0.468 0.814 0.467 !       1.87 eA-3
C120 0.601 0.109 0.008 !       1.84 eA-3
C121 0.535 0.091 0.039 !       1.77 eA-3
C122 0.485 0.742 0.007 !       1.74 eA-3
C123 0.421 0.937 0.024 !       1.72 eA-3
C124 0.453 0.614 0.354 !       1.69 eA-3
C125 0.343 0.794 0.032 !       1.68 eA-3
C126 0.494 0.079 0.118 !       1.68 eA-3
C127 0.532 0.046 0.093 !       1.67 eA-3
C128 0.414 0.859 0.024 !       1.65 eA-3
C129 0.466 0.701 0.357 !       1.64 eA-3
C130 0.601 0.095 0.050 !       1.55 eA-3
C131 0.545 0.257 0.068 !       1.54 eA-3
C132 0.443 0.716 0.085 !       1.49 eA-3
C133 0.466 0.091 0.041 !       1.47 eA-3
C134 0.391 0.980 0.046 !       1.44 eA-3
C135 0.461 0.450 0.499 !       1.36 eA-3
C136 0.451 0.953 0.045 !       1.36 eA-3
C137 0.336 0.794 0.009 !       1.36 eA-3
C138 0.500 0.081 0.070 !       1.35 eA-3
Q139 0.599 0.190 0.163 !       1.34 eA-3
C140 0.652 0.133 0.109 !       1.33 eA-3
C141 0.517 0.466 0.492 !       1.33 eA-3
C142 0.456 0.592 0.435 !       1.32 eA-3
C143 0.503 0.080 0.018 !       1.31 eA-3
C144 0.388 0.764 0.477 !       1.28 eA-3
C145 0.528 0.358 0.446 !       1.27 eA-3
Q146 0.460 0.360 0.492 !       1.26 eA-3
Q147 0.516 0.831 0.453 !       1.25 eA-3
C148 0.538 0.689 0.445 !       1.23 eA-3
C149 0.444 0.027 0.058 !       1.20 eA-3
Q150 0.459 0.813 0.109 !       1.17 eA-3
C151 0.585 0.466 0.423 !       1.16 eA-3
C152 0.589 0.059 0.110 !       1.16 eA-3
Q153 0.604 0.421 0.407 !       1.16 eA-3
Q154 0.505 0.330 0.068 !       1.15 eA-3
Q155 0.285 0.155 0.110 !       1.14 eA-3
C156 0.461 0.732 0.047 !       1.13 eA-3
C157 0.421 0.703 0.040 !       1.13 eA-3
C158 0.667 0.474 0.476 !       1.12 eA-3
C159 0.650 0.215 0.446 !       1.11 eA-3
C160 0.344 0.703 0.019 !       1.09 eA-3
Q161 0.360 0.969 0.063 !       1.04 eA-3
Q162 0.605 0.329 0.399 !       1.04 eA-3
Q163 0.501 0.982 0.117 !       1.04 eA-3
Q164 0.153 0.750 0.196 !       1.03 eA-3
Q165 0.713 0.355 0.491 !       1.01 eA-3
C166 0.550 0.017 0.040 !       1.00 eA-3
C167 0.629 0.065 0.087 !       0.99 eA-3
Q168 0.329 0.627 0.008 !       0.97 eA-3
Q169 0.318 0.638 0.359 !       0.97 eA-3
Q170 0.356 0.059 0.123 !       0.97 eA-3
Q171 0.685 0.547 0.388 !       0.96 eA-3
C172 0.505 0.231 0.413 !       0.96 eA-3
C173 0.618 0.172 0.416 !       0.96 eA-3
C174 0.542 0.264 0.126 !       0.95 eA-3
C175 0.502 0.155 0.501 !       0.93 eA-3
C176 0.469 0.014 0.037 !       0.92 eA-3
C177 0.484 0.485 0.429 !       0.92 eA-3
Q178 0.640 0.390 0.439 !       0.92 eA-3
C179 0.645 0.297 0.063 !       0.91 eA-3
Q180 0.480 0.968 0.423 !       0.91 eA-3
Q181 0.511 0.849 0.102 !       0.91 eA-3
Q182 0.595 0.581 0.009 !       0.90 eA-3
Q183 0.343 0.185 0.112 !       0.90 eA-3
Q184 0.338 0.796 0.077 !       0.89 eA-3
Q185 0.484 0.577 0.084 !       0.89 eA-3
C186 0.321 0.639 0.429 !       0.89 eA-3
C187 0.452 0.217 0.140 !       0.88 eA-3
Q188 0.446 0.517 0.365 !       0.87 eA-3
C189 0.676 0.327 0.040 !       0.87 eA-3
Q190 0.726 0.091 0.102 !       0.87 eA-3
Q191 0.358 0.767 0.087 !       0.86 eA-3
Q192 0.527 0.777 0.063 !       0.86 eA-3
C193 0.497 0.917 0.039 !       0.86 eA-3
Q194 0.353 0.496 0.454 !       0.86 eA-3
C195 0.452 0.202 0.103 !       0.86 eA-3
Q196 0.542 0.939 0.049 !       0.86 eA-3
C197 0.586 0.543 0.490 !       0.85 eA-3
C198 0.500 0.643 0.336 !       0.84 eA-3
Q199 0.557 0.609 0.406 !       0.84 eA-3
;
_refine_diff_density_max         0.782
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         8752
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.2089
_refine_ls_R_factor_gt           0.1270
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1188P)^2^+56.9326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2735
_refine_ls_wR_factor_ref         0.3143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5067
_reflns_number_total             8752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02833_si_005.cif
_cod_data_source_block           14_a_sqd
_cod_database_code               4345443
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.864
_shelx_estimated_absorpt_t_max   0.864
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              1698
_shelx_hkl_checksum              76859