Electrochemical synthesis and crystal structure studies of defective dicubane tetranuclear hydroxo and carboxamide ligand bridged cobalt(II)–cobalt(III) complexes with carboxamides produced from unprotected hydroxyaromatic carboxylic acids
Meghdadi, Soraia; Mirkhani, Valiollah; Mereiter, Kurt; Comptes Rendus Chimie 18 (2015) 654–661; doi:10.1016/j.crci.2014.11.001

data_1566123
_publ_section_title
;
 Electrochemical synthesis and crystal structure studies of defective
 dicubane tetranuclear hydroxo and carboxamide ligand bridged
 cobalt(II)--cobalt(III) complexes with carboxamides produced from
 unprotected hydroxyaromatic carboxylic acids
;
_journal_issue                   6
_journal_name_full               'Comptes Rendus Chimie'
_journal_page_first              654
_journal_page_last               661
_journal_paper_doi               10.1016/j.crci.2014.11.001
_journal_volume                  18
_journal_year                    2015
_chemical_formula_moiety         'C56 H52 Co4 N10 O10, 2(H2 O), 2(C2 H3 N)'
_chemical_formula_sum            'C60 H62 Co4 N12 O12'
_chemical_formula_weight         1378.94
_chemical_name_common
;
1598 SM2prime [Co4(\m3-OH)2(\m2-Me2hybeb)2(CH3CN)6].2H2O.2(CH3CN)
;
_chemical_name_systematic
; 
[Co4(\m3-OH)2(\m2-Me2hybeb)2(CH3CN)6].2H2O.2(CH3CN)
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.574(3)
_cell_angle_beta                 63.112(3)
_cell_angle_gamma                85.976(3)
_cell_formula_units_Z            1
_cell_length_a                   12.0549(6)
_cell_length_b                   12.4484(6)
_cell_length_c                   12.7005(6)
_cell_measurement_reflns_used    3807
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.90
_cell_measurement_theta_min      2.44
_cell_volume                     1531.60(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'MERCURY  (Macrae et al., 2006)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_sigmaI/netI    0.080
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16757
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             710
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
TITL 1598squeeze with program PLATON    R = 0.06
CELL   12.0549   12.4484   12.7005     65.57     63.11     85.98
SPGR P-1
C101 0.240 0.425 0.897 !       6.57 eA-3
C102 0.207 0.606 0.982 !       5.67 eA-3
C103 0.093 0.531 0.018 !       3.53 eA-3
C104 0.785 0.470 0.061 !       3.53 eA-3
C105 0.840 0.506 0.047 !       3.45 eA-3
Q106 0.538 0.718 0.465 !       2.35 eA-3
Q107 0.609 0.463 0.541 !       2.24 eA-3
Q108 0.312 0.115 0.515 !       1.42 eA-3
C109 0.982 0.594 0.030 !       1.36 eA-3
Q110 0.469 0.968 0.385 !       1.30 eA-3
;
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         5127
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1575
_reflns_number_gt                3398
_reflns_number_total             5127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            CRC-2015-18-654.cif
_cod_data_source_block           1598
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_cell_volume        1531.60(13)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               1566123