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_7702063
_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 H48 Br4 Co4 N4 O14, O, 2(C H3 O)'
_chemical_formula_sum            'C44 H54 Br4 Co4 N4 O17'
_chemical_formula_weight         1466.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-23 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.388(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1056(4)
_cell_length_b                   11.7616(2)
_cell_length_c                   27.3199(8)
_cell_measurement_reflns_used    5196
_cell_measurement_temperature    125.40(14)
_cell_measurement_theta_max      28.7160
_cell_measurement_theta_min      3.7810
_cell_volume                     5324.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      125.40(14)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.9983
_diffrn_measurement_details
;
  1 omega   -5.00   56.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  -99.0000 -120.0000 61

  2 omega   34.00   86.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497   63.0000  -61.0000 52

  3 omega  -28.00   45.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  -19.0000  -30.0000 73

  4 omega    1.00   59.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  -99.0000  120.0000 58
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0210827000
_diffrn_orient_matrix_UB_12      0.0369335000
_diffrn_orient_matrix_UB_13      0.0127906000
_diffrn_orient_matrix_UB_21      -0.0073067000
_diffrn_orient_matrix_UB_22      -0.0461335000
_diffrn_orient_matrix_UB_23      0.0149748000
_diffrn_orient_matrix_UB_31      0.0365324000
_diffrn_orient_matrix_UB_32      0.0120941000
_diffrn_orient_matrix_UB_33      0.0181708000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13100
_diffrn_reflns_theta_full        25.0095
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.298
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.8292
_exptl_crystal_description       prism
_exptl_crystal_F_000             2922.6677
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.8117
_refine_diff_density_min         -0.7686
_refine_diff_density_rms         0.1141
_refine_ls_d_res_high            0.8406
_refine_ls_d_res_low             7.0568
_refine_ls_goodness_of_fit_ref   1.0662
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    41
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4688
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.0660
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+22.4461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              -20
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                4084
_reflns_number_total             4688
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt00380j2.cif
_cod_data_source_block           P150509F
_cod_original_sg_symbol_Hall     '-C 2yc (x,y,-x+z)'
_cod_database_code               7702063
_chemical_oxdiff_formula         C1H1O1N1CO1
_chemical_oxdiff_usercomment     C8
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 O7-H7
 0.85 with sigma of 0.01
 C21-H7
 1.8832 with sigma of 0.02
3. Others
 Fixed Sof: Br0a(0.5) Br1(0.5)
4.a Ternary CH refined with riding coordinates:
 C10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C9(H9a,H9b)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C6(H6), C4(H4), C8(H8), C16(H16), C12(H12)
4.d Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C1(H1a,H1b,H1c), C22(H22a,H22b,H22c), C20(H20a,H20b,
 H20c), C21(H21a,H21b,H21c)
;
_olex2_submission_special_instructions 'No special instructions were received'