Charge density studies of 3<i>d</i> metal (Ni/Cu) complexes with a non-innocent ligand
Chuang, Yu-Chun; Sheu, Chou-Fu; Lee, Gene-Hsiang; Chen, Yu-Sheng; Wang, Yu; Acta Crystallographica Section B 73 (2017) 634–642; doi:10.1107/S2052520617007119

data_2108134
_publ_section_title
;
 Charge density studies of 3<i>d</i> metal (Ni/Cu) complexes with a
 non-innocent ligand
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              634
_journal_page_last               642
_journal_paper_doi               10.1107/S2052520617007119
_journal_volume                  73
_journal_year                    2017
_chemical_formula_sum            'C13 H6 N5 Ni S4'
_chemical_formula_weight         419.18
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.837(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1805(10)
_cell_length_b                   6.3567(5)
_cell_length_c                   17.0872(7)
_cell_measurement_reflns_used    16292
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.00
_cell_measurement_theta_min      1.41
_cell_volume                     1568.20(18)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0119
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16292
_diffrn_reflns_theta_full        50.00
_diffrn_reflns_theta_max         50.00
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    1.773
_exptl_absorpt_correction_T_max  0.7182
_exptl_absorpt_correction_T_min  0.5026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.470
_refine_ls_extinction_coef       0.0065(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         16292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+0.3858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                14166
_reflns_number_total             16292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            lc5076sup1.cif
_cod_data_source_block           CCDC_1525430
_cod_original_cell_volume        1568.20(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2108134
_cod_database_fobs_code 2108134