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_2108888
_publ_section_title
;
 Self-assembling of three rare structurally various homomultinuclear
 Cu^II^ complexes derived from a bis(salamo)-based multioxime ligand
;
_journal_coeditor_code           LO5094
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520621008441
_journal_volume                  77
_journal_year                    2021
_chemical_formula_moiety         'C56 H54 Cu4 N12 O24, 2(Cl O4), 2(C H4 O)'
_chemical_formula_sum            'C58 H62 Cl2 Cu4 N12 O34'
_chemical_formula_weight         1796.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-01 # Formatted by IUCr publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 92.0860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2568(4)
_cell_length_b                   14.5155(4)
_cell_length_c                   15.4550(4)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.726
_cell_measurement_theta_min      2.370
_cell_volume                     3420.40(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_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  0.0243
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43196
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.736
_diffrn_reflns_theta_min         2.316
_exptl_absorpt_coefficient_mu    1.410
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.759
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7259
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0340P)^2^+5.5923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6759
_reflns_number_total             7259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5094sup1.cif
_cod_data_source_block           1
_cod_database_code               2108888
_publcif_datablock.id            {5eabb18f-54b1-4433-8338-9f6c38726244}
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.775
_shelx_estimated_absorpt_t_min   0.728
_olex2_refinement_description
;
1. 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 C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O12-H12
 0.87 with sigma of 0.01
 C28-H12
 1.899022 with sigma of 0.02
 Cu2-H12
 2.830607 with sigma of 0.02
 O14-Cl1 \\sim Cl1-O14A
 with sigma of 0.02
 O15A-Cl1 \\sim Cl1-O15
 with sigma of 0.02
 O13A-C29 \\sim C29-O13
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O13A \\sim O14 \\sim O14A: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(O13A)=Sof(H13A)=Sof(O14A)=Sof(O15A)=Sof(H29d)=Sof(H29e)=Sof(H29f)=1-FVAR(1)
 Sof(O13)=Sof(H13)=Sof(O14)=Sof(O15)=Sof(H29a)=Sof(H29b)=Sof(H29c)=FVAR(1)
5.a Riding coordinates:
 O13(H13), O13A(H13A)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b), C19(H19a,H19b), C20(H20a,H20b)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C14(H14), C16(H16), C18(H18),
 C21(H21), C24(H24), C25(H25), C27(H27)
5.d Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C28(H28a,H28b,H28c), C29(H29a,H29b,H29c), C29(H29d,H29e,
 H29f)
;
_shelx_res_checksum              5182
_shelx_hkl_checksum              98348
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2108888