Tetranuclear and dinuclear phenoxido bridged copper complexes based on unsymmetrical thiosemicarbazone ligands.
Isaac, J. A.; Mansour, A.-T.; David, R.; Kochem, A.; Philouze, C.; Demeshko, S.; Meyer, F.; Réglier, M; Simaan, A. J.; Caldarelli, S.; Yemloul, M.; Jamet, H.; Thibon-Pourret, A; Belle, C.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9665–9676; doi:10.1039/c8dt02452a

data_7046889
_publ_section_title
;
 Tetranuclear and dinuclear phenoxido bridged copper complexes based on
 unsymmetrical thiosemicarbazone ligands.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9665
_journal_page_last               9676
_journal_paper_doi               10.1039/c8dt02452a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C46 H50 Cu4 N12 O4 S2, 2(C F3 O3 S), 3(C2 H3 N)'
_chemical_formula_sum            'C54 H59 Cu4 F6 N15 O10 S4'
_chemical_formula_weight         1574.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2016-12-01 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.964(7)
_cell_length_b                   14.683(3)
_cell_length_c                   14.437(3)
_cell_measurement_reflns_used    47707
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.999
_cell_measurement_theta_min      2.775
_cell_volume                     6439(3)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Incoatec-Bruker-AXS-enraf-noniusKappaAPEXII
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47707
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.775
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.648116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1829 before and 0.0548 after correction.
The Ratio of minimum to maximum transmission is 0.6481.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       prism
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         9332
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0355P)^2^+12.4887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6291
_reflns_number_total             9332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02452a2.cif
_cod_data_source_block           nanny
_cod_depositor_comments
'Adding full bibliography for 7046887--7046889.cif.'
_cod_database_code               7046889
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-C28
 1.45 with sigma of 0.02
 N8-C27
 1.2 with sigma of 0.02
3. Rigid bond restraints
 C27, C28, N8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C27 \\sim C28 \\sim N8: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
5. Others
 Fixed Sof: C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) N8(0.5) C27(0.5)
6.a Rotating group:
 O2(H2)
6.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C8(H8A,H8B), C12(H12A,H12B)
6.c Aromatic/amide H refined with riding coordinates:
 N6(H6), C7(H7), C14(H14), C17(H17), C5(H5), C22(H22), C3(H3), C20(H20),
 C15(H15), C16(H16), C21(H21), C23(H23)
6.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              97452
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'