Crystal structure of (1,10-phenanthroline-κ2 N,N′)-bis(3-thiophenecarboxylato-κ2 O,O′)copper(II), C22H14N2O4S2Cu
Zhang, Zhongyu; Men, Xiaoxia; Han, Bing; Sun, Chunyan; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 1019–1020; doi:10.1515/ncrs-2021-0199

data_8104654
_publ_section_title
;
 Crystal structure of (1,10-phenanthroline-\k2
 N,N&#x2032;)-bis(3-thiophenecarboxylato-\k2 O,O&#x2032;)copper(II),
 C22H14N2O4S2Cu
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1019
_journal_page_last               1020
_journal_paper_doi               10.1515/ncrs-2021-0199
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C22 H14 Cu N2 O4 S2'
_chemical_formula_sum            'C22 H14 Cu N2 O4 S2'
_chemical_formula_weight         498.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.171(7)
_cell_length_b                   9.684(3)
_cell_length_c                   10.372(4)
_cell_measurement_reflns_used    5428
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.020
_cell_measurement_theta_min      2.333
_cell_volume                     2026.0(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker APEX-II&#x00EF;&#x00BC;&#x008C;CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12036
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.032
_diffrn_reflns_theta_min         2.333
_exptl_absorpt_coefficient_mu    1.318
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0680 before and 0.0355 after correction. The Ratio of minimum to maximum transmission is 0.8104. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2003
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+1.6105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1737
_reflns_number_total             2003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0199_suppl.cif
_cod_data_source_block           1_a
_cod_original_cell_volume        2025.9(12)
_cod_database_code               8104654
_shelx_estimated_absorpt_t_max   0.779
_shelx_estimated_absorpt_t_min   0.693
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 S1-C3 = S1A-C5
 1.705 with sigma of 0.01
 S1-C4 = S1A-C4A
 1.665 with sigma of 0.01
 C4-C5 = C4A-C3
 1.414 with sigma of 0.01
 S1-C5 = S1A-C3
 2.528 with sigma of 0.01
 C4-C3 = C4A-C5
 2.459 with sigma of 0.01
3. Rigid bond restraints
 C2, C3, C4, C5, C4A, S1, S1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C4A \\sim S1 \\sim S1A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) = Uanis(C4A)
Uanis(O1) = Uanis(O2)
5. Others
 Sof(S1A)=Sof(C4A)=Sof(H4A)=1-FVAR(1)
 Sof(S1)=Sof(C4)=Sof(H4)=FVAR(1)
6.a Riding coordinates:
 C3(H3), C5(H5)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C8(H8), C11(H11), C4A(H4A)
;