Synthesis, magnetism and spectral studies of six defective dicubane tetranuclear {M4O6} (M = Ni(II), Co(II), Zn(II)) and three trinuclear Cd(II) complexes with polydentate Schiff base ligands.
Jiang, Lin; Zhang, Dong-Yan; Suo, Jing-Jing; Gu, Wen; Tian, Jin-Lei; Liu, Xin; Yan, Shi-Ping; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10233–10248; doi:10.1039/c6dt00380j

data_7702067
_publ_section_title
;
 Synthesis, magnetism and spectral studies of six defective dicubane
 tetranuclear {M4O6} (M = Ni(II), Co(II), Zn(II)) and three trinuclear
 Cd(II) complexes with polydentate Schiff base ligands.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10233
_journal_page_last               10248
_journal_paper_doi               10.1039/c6dt00380j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C42 H42 Br4 Cd3 N4 O14, C H4 O'
_chemical_formula_sum            'C43 H46 Br4 Cd3 N4 O15'
_chemical_formula_weight         1515.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-21 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 116.57(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.133(3)
_cell_length_b                   15.107(3)
_cell_length_c                   24.295(9)
_cell_measurement_temperature    293(2)
_cell_volume                     5296(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9321
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.85
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.277
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         9321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+5.1856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                7581
_reflns_number_total             9321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00380j2.cif
_cod_data_source_block           cdde_sq_d
_cod_original_cell_volume        5296(2)
_cod_database_code               7702067
_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
2. Others
 Fixed Sof: Br7(0.5) Br1(0.5)
3.a Ternary CH refined with riding coordinates:
 C10(H10), C29(H29)
3.b Secondary CH2 refined with riding coordinates:
 C28(H28a,H28b), C9(H9a,H9b), C11(H11a,H11b), C30(H30a,H30b)
3.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C35(H35), C23(H23), C25(H25), C6(H6), C8(H8a), C27(H27), C4(H4),
 C14(H14), C12(H12), C31(H31), C33(H33)
3.d Idealised Me refined as rotating group:
 C40(H40a,H40b,H40c), C38(H38a,H38b,H38c), C42(H42a,H42b,H42c), C20(H20a,H20b,
 H20c), C19(H19a,H19b,H19c), C1(H1a,H1b,H1c), C43(Ha,Hb,Hc)
3.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O8(H8), O15(H)
;
_olex2_submission_special_instructions 'No special instructions were received'