Self-assembling of three rare structurally various homomultinuclear Cu^II^ complexes derived from a bis(salamo)-based multioxime ligand
Li, Peng; Zhang, Ting; Li, Li-Li; Dong, Wen-Kui; Acta Crystallographica Section B 77 (2021) –; doi:10.1107/S2052520621008441

data_2108890
_publ_section_title
;
 Self-assembling of three rare structurally various homomultinuclear
 Cu^II^ complexes derived from a bis(salamo)-based multioxime ligand
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
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;
_journal_paper_doi               10.1107/S2052520621008441
_journal_volume                  77
_journal_year                    2021
_chemical_formula_moiety         'C29 H30 Br2 Cu2 N6 O12, C H Cl3'
_chemical_formula_sum            'C30 H31 Br2 Cl3 Cu2 N6 O12'
_chemical_formula_weight         1060.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-12-05
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_cell_angle_alpha                90
_cell_angle_beta                 101.859(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3330(4)
_cell_length_b                   17.1049(4)
_cell_length_c                   16.3502(5)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.72
_cell_measurement_theta_min      2.38
_cell_volume                     3922.93(19)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35876
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.784
_diffrn_reflns_theta_min         2.381
_exptl_absorpt_coefficient_mu    3.392
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.023(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         8303
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0373P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.987
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                7711
_reflns_number_total             8303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5094sup1.cif
_cod_data_source_block           3
_cod_database_code               2108890
_publcif_datablock.id            {150a5e8f-cf0a-41b9-955a-b5b6fde68a37}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.509
_shelx_estimated_absorpt_t_min   0.473
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.977(8)
 0.023(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 O12-H12
 0.87 with sigma of 0.01
 C29-H12
 1.927642 with sigma of 0.02
 Cu1-H12
 2.896065 with sigma of 0.02
 Cl2-C30 \\sim Cl0A-C30
 with sigma of 0.02
 Cl2A-C30A \\sim Cl3-C30A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Cl0A \\sim Cl1 \\sim Cl1A \\sim Cl2 \\sim Cl2A \\sim Cl3: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C30A, Cl1A, Cl2A, Cl3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30, Cl0A, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C30A)=Sof(H30A)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3)=1-FVAR(1)
 Sof(C30)=Sof(H30)=Sof(Cl0A)=Sof(Cl1)=Sof(Cl2)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C30(H30), C30A(H30A)
7.b Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b), C19(H19a,H19b), C20(H20a,H20b), C29(H29a,H29b)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C10(H10), C14(H14), C16(H16), C18(H18),
 C21(H21), C24(H24), C25(H25), C27(H27)
7.d Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C28(H28a,H28b,H28c)
7.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_shelx_res_checksum              92441
_shelx_hkl_checksum              56429
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_info_exptl_table_max_cols 5
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
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_cod_database_fobs_code 2108890