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_7046887
_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         'C23 H26 N6 O S'
_chemical_formula_sum            'C23 H26 N6 O S'
_chemical_formula_weight         434.56
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-12-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2017-01-04 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.92(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.911(2)
_cell_length_b                   18.212(4)
_cell_length_c                   12.793(3)
_cell_measurement_reflns_used    28560
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.95
_cell_volume                     2300.6(9)
_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-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            KappaCCD
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaCCD'
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28560
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         1.950
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.373067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.2585 before and 0.0491 after correction.
The Ratio of minimum to maximum transmission is 0.3731.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         5022
_refine_ls_number_restraints     844
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0448P)^2^+0.8940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3224
_reflns_number_total             5022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02452a2.cif
_cod_data_source_block           sad2
_cod_depositor_comments
'Adding full bibliography for 7046887--7046889.cif.'
_cod_original_cell_volume        2300.8(8)
_cod_database_code               7046887
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All S(H) groups
2. Restrained distances
 C2-C8
 1.4 with sigma of 0.02
 C3-C2
 1.4 with sigma of 0.02
 C2'-C8
 1.4 with sigma of 0.02
 C1-C2'
 1.4 with sigma of 0.02
 C10-N6
 1.35 with sigma of 0.02
 C10'-N6'
 1.35 with sigma of 0.02
 N3-C10
 1.3 with sigma of 0.02
 N3'-C10'
 1.3 with sigma of 0.02
3. Rigid bond restraints
 C5', C18, C9, C11, N4, C21, C16', C16, C15', C12, N6', C22, C1, C13, C4', N2',
  N3, C21', C7', N6, C19, O1, C2', C11', C9', N5', C15, C3, C4, N2, C20', C6,
 C7, C2, N4', C23', C6', C14, C10, N1, C20, C3', C17', C23, C17, S1, S1', C5,
 N5, C8, N3', C10', C14'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C5' \\sim C18 \\sim C9 \\sim C11 \\sim N4 \\sim C21 \\sim C16' \\sim C16 \\sim
C15' \\sim C12 \\sim N6' \\sim C22 \\sim C1 \\sim C13 \\sim C4' \\sim N2' \\sim
N3 \\sim C21' \\sim C7' \\sim N6 \\sim C19 \\sim O1 \\sim C2' \\sim C11' \\sim
C9' \\sim N5' \\sim C15 \\sim C3 \\sim C4 \\sim N2 \\sim C20' \\sim C6 \\sim C7
\\sim C2 \\sim N4' \\sim C23' \\sim C6' \\sim C14 \\sim C10 \\sim N1 \\sim C20
\\sim C3' \\sim C17' \\sim C23 \\sim C17 \\sim S1 \\sim S1' \\sim C5 \\sim N5
\\sim C8 \\sim N3' \\sim C10' \\sim C14': within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C11') \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C11) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
5. Others
 Sof(S1')=Sof(N3')=Sof(H3')=Sof(N6')=Sof(H6')=Sof(C4')=Sof(C2')=Sof(C6')=
 Sof(C3')=Sof(H3'A)=Sof(H8BC)=Sof(H8BD)=Sof(C5')=Sof(H5')=Sof(C9')=Sof(H9'A)=
 Sof(H9'B)=Sof(H9'C)=Sof(C11')=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(N2')=Sof(C7')=
 Sof(H7')=Sof(C10')=1-FVAR(1)
 Sof(C10)=Sof(N2)=Sof(H8AA)=Sof(H8AB)=Sof(C7)=Sof(H7)=Sof(C11)=Sof(H11A)=
 Sof(H11B)=Sof(H11C)=Sof(C5)=Sof(H5)=Sof(C3)=Sof(H3)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(H9C)=Sof(C6)=Sof(C4)=Sof(N6)=Sof(H6)=Sof(N3)=Sof(C2)=Sof(S1)=Sof(H1A)=
 FVAR(1)
 Sof(H22A)=Sof(C20')=Sof(H20')=Sof(C21')=Sof(H21')=Sof(N5')=Sof(C23')=
 Sof(H23')=1-FVAR(2)
 Sof(H22)=Sof(N5)=Sof(C23)=Sof(H23)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=FVAR(2)
 Sof(C14')=Sof(H14')=Sof(C16')=Sof(H16')=Sof(C17')=Sof(H17')=Sof(N4')=
 Sof(C15')=Sof(H15')=1-FVAR(3)
 Sof(N4)=Sof(C17)=Sof(H17)=Sof(C16)=Sof(H16)=Sof(C15)=Sof(H15)=Sof(C14)=
 Sof(H14)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C8(H8BC,H8BD), C8(H8AA,H8AB), C18(H18A,H18B)
6.b Aromatic/amide H refined with riding coordinates:
 N3'(H3'), N6'(H6'), C3'(H3'A), C7(H7), C5'(H5'), C14'(H14'), C17(H17),
 C22(H22A), C22(H22), C16(H16), C15(H15), C20'(H20'), C21'(H21'), C23(H23),
 C20(H20), C23'(H23'), C21(H21), C5(H5), C3(H3), N6(H6), C7'(H7'), C16'(H16'),
 C14(H14), C17'(H17'), C15'(H15')
6.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C9'(H9'A,H9'B,H9'C), C9(H9A,H9B,H9C), C11'(H11D,H11E,H11F)
6.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), S1(H1A)
;
_shelx_res_checksum              68274
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'