#------------------------------------------------------------------------------
#$Date: 2024-07-05 19:42:27 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293112 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/57/7715751.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7715751
loop_
_publ_author_name
'Geoghegan, Blaise L.'
'Bilyj, Jessica K.'
'Bernhardt, Paul V.'
'DeBeer, Serena'
'Cutsail, 3rd, George E'
_publ_section_title
;
 X-ray absorption and emission spectroscopy of N₂S₂
 Cu(II)/(III) complexes.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7828
_journal_page_last               7838
_journal_paper_doi               10.1039/d4dt00085d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C21 H21 Cu N4 S4'
_chemical_formula_weight         521.2
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_creation_date             2022-07-14T17:20:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2022-09-01 deposited with the CCDC.	2024-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.058(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8933(4)
_cell_length_b                   8.90930(10)
_cell_length_c                   10.5529(2)
_cell_measurement_reflns_used    3828
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      61.43
_cell_measurement_theta_min      5.29
_cell_measurement_wavelength     1.54184
_cell_volume                     2218.41(6)
_computing_cell_refinement       'CrysalisPro (Agilent Technologies,     )'
_computing_data_collection       'CrysalisPro (Agilent Technologies,     )'
_computing_data_reduction        'CrysalisPro (Agilent Technologies,     )'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      190(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.02
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type
'Agilent Technologies Xcalibur, EosS2, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.02505
_diffrn_orient_matrix_UB_12      0.140522
_diffrn_orient_matrix_UB_13      -0.055042
_diffrn_orient_matrix_UB_21      0.005127
_diffrn_orient_matrix_UB_22      -0.086857
_diffrn_orient_matrix_UB_23      -0.123836
_diffrn_orient_matrix_UB_31      -0.060092
_diffrn_orient_matrix_UB_32      0.051292
_diffrn_orient_matrix_UB_33      -0.058878
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5249
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        61.567
_diffrn_reflns_theta_max         61.567
_diffrn_reflns_theta_min         3.747
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.039
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.778
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0885P)²+9.6077P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1677
_reflns_Friedel_coverage         0
_reflns_number_gt                1638
_reflns_number_total             1720
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00085d2.cif
_cod_data_source_block           2248jbc7
_cod_depositor_comments
'Adding full bibliography for 7715751--7715752.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7715751
_shelx_estimated_absorpt_t_min   0.238
_shelx_estimated_absorpt_t_max   0.824
_shelx_shelxl_version_number     2018/1
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'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5 0.8582(7) 0.75 0.0519(17) Uani 1 2 d S T P . .
H1 H 0.499999 0.964788 0.749997 0.062 Uiso 1 2 calc R U P . .
C2 C 0.53396(17) 0.7902(5) 0.6691(5) 0.0507(12) Uani 1 1 d . . . . .
C3 C 0.5658(2) 0.8895(5) 0.5895(6) 0.0627(15) Uani 1 1 d . . . . .
H3A H 0.60661 0.880565 0.619863 0.094 Uiso 1 1 calc R U . . .
H3B H 0.554054 0.994015 0.597369 0.094 Uiso 1 1 calc R U . . .
H3C H 0.557546 0.858549 0.499335 0.094 Uiso 1 1 calc R U . . .
C4 C 0.58150(18) 0.4473(6) 0.5824(5) 0.0474(11) Uani 1 1 d . . . . .
C5 C 0.6667(2) 0.5094(6) 0.4349(4) 0.0504(12) Uani 1 1 d . . . . .
H5A H 0.678989 0.481426 0.352715 0.06 Uiso 1 1 calc R U . . .
H5B H 0.642827 0.600342 0.419398 0.06 Uiso 1 1 calc R U . . .
C6 C 0.71803(18) 0.5461(5) 0.5307(4) 0.0381(9) Uani 1 1 d . . . . .
C7 C 0.71681(19) 0.6625(5) 0.6183(4) 0.0419(10) Uani 1 1 d . . . . .
H7 H 0.682848 0.717849 0.618466 0.05 Uiso 1 1 calc R U . . .
C8 C 0.7645(2) 0.6982(5) 0.7051(4) 0.0449(10) Uani 1 1 d . . . . .
H8 H 0.7634 0.778291 0.764026 0.054 Uiso 1 1 calc R U . . .
C9 C 0.8136(2) 0.6178(6) 0.7059(4) 0.0499(11) Uani 1 1 d . . . . .
H9 H 0.846233 0.641451 0.766231 0.06 Uiso 1 1 calc R U . . .
C10 C 0.8155(2) 0.5025(5) 0.6192(5) 0.0493(12) Uani 1 1 d . . . . .
H10 H 0.849542 0.447211 0.619718 0.059 Uiso 1 1 calc R U . . .
C11 C 0.76827(19) 0.4676(5) 0.5322(4) 0.0444(10) Uani 1 1 d . . . . .
H11 H 0.770036 0.388799 0.472343 0.053 Uiso 1 1 calc R U . . .
Cu1 Cu 0.5 0.50093(9) 0.75 0.0408(4) Uani 1 2 d S T P . .
N1 N 0.53915(15) 0.6414(4) 0.6620(4) 0.0492(10) Uani 1 1 d . . . . .
N2 N 0.57673(15) 0.5919(4) 0.5844(4) 0.0480(10) Uani 1 1 d . . . . .
S1 S 0.54721(7) 0.32525(14) 0.67214(19) 0.0795(6) Uani 1 1 d . . . . .
S2 S 0.62404(5) 0.35705(14) 0.48496(13) 0.0539(4) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C2 C1 C2 128.9(6) 2_656 . ?
N1 C2 C1 122.0(5) . . ?
N1 C2 C3 119.5(4) . . ?
C1 C2 C3 118.5(4) . . ?
N2 C4 S1 124.5(4) . . ?
N2 C4 S2 121.8(4) . . ?
S1 C4 S2 113.7(3) . . ?
C6 C5 S2 113.7(3) . . ?
C11 C6 C7 118.4(4) . . ?
C11 C6 C5 120.9(4) . . ?
C7 C6 C5 120.7(4) . . ?
C8 C7 C6 120.6(4) . . ?
C9 C8 C7 119.9(4) . . ?
C8 C9 C10 120.1(5) . . ?
C11 C10 C9 120.1(5) . . ?
C10 C11 C6 120.8(4) . . ?
N1 Cu1 N1 97.1(2) . 2_656 ?
N1 Cu1 S1 87.97(12) . . ?
N1 Cu1 S1 172.76(14) 2_656 . ?
N1 Cu1 S1 172.76(14) . 2_656 ?
N1 Cu1 S1 87.97(12) 2_656 2_656 ?
S1 Cu1 S1 87.43(8) . 2_656 ?
C2 N1 N2 115.2(4) . . ?
C2 N1 Cu1 124.9(3) . . ?
N2 N1 Cu1 119.9(3) . . ?
C4 N2 N1 113.2(4) . . ?
C4 S1 Cu1 94.19(17) . . ?
C4 S2 C5 103.4(2) . . ?
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
C1 C2 1.404(6) 2_656 ?
C1 C2 1.404(6) . ?
C2 N1 1.335(6) . ?
C2 C3 1.507(7) . ?
C4 N2 1.294(6) . ?
C4 S1 1.730(5) . ?
C4 S2 1.751(5) . ?
C5 C6 1.497(6) . ?
C5 S2 1.825(5) . ?
C6 C11 1.387(6) . ?
C6 C7 1.393(6) . ?
C7 C8 1.383(6) . ?
C8 C9 1.372(7) . ?
C9 C10 1.382(7) . ?
C10 C11 1.373(7) . ?
Cu1 N1 1.891(4) . ?
Cu1 N1 1.891(4) 2_656 ?
Cu1 S1 2.1655(15) . ?
Cu1 S1 2.1655(15) 2_656 ?
N1 N2 1.380(5) . ?
