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_7046888
_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         'C24 H27 Cu2 N6 O2 S, C F3 O3 S, H2 O'
_chemical_formula_sum            'C25 H29 Cu2 F3 N6 O6 S2'
_chemical_formula_weight         757.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-11-17
_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                95.74(3)
_cell_angle_beta                 95.74(3)
_cell_angle_gamma                92.90(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7438(17)
_cell_length_b                   10.771(2)
_cell_length_c                   15.739(3)
_cell_measurement_reflns_used    36785
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.998
_cell_measurement_theta_min      2.421
_cell_volume                     1464.7(5)
_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-2016 (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            KappaCCD
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0855
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36785
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.421
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.665
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.600376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.3587 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.6004.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       needle
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         8473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0776P)^2^+0.5783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5712
_reflns_number_total             8473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02452a2.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7046887--7046889.cif.'
_cod_database_code               7046888
_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 O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O6(H6A,H6B)
2.b Rotating group:
 O2(H2)
2.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C19(H19A,H19B), C8(H8A,H8B)
2.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C3(H3), C22(H22), C24(H24), C5(H5), C15(H15), C16(H16), C17(H17),
 C21(H21), C7(H7), C23(H23)
2.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              25634
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'