Three p-tert-Butylthiacalix[4]arene-Supported Cobalt Compounds Obtained in One Pot Involving In Situ Formation of N6H2 Ligand
Yanfeng Bi; Wuping Liao; Guancheng Xu; Ruiping Deng; Meiyan Wang; Zhijian Wu; Song Gao; Hongjie Zhang; Inorganic Chemistry 49 (2010) 7735–7740; doi:10.1021/ic1005105

data_4316345
_publ_contact_author             'Prof Dr Wuping Liao'
_publ_contact_author_address
;     State Key Lab of Rare Earth Resource Utilization
      Changchun Institute of Applied Chemistry
      CAS, Changchun 130022
      P.R. China
;
_publ_contact_author_email       wpliao@ciac.jl.cn
_publ_section_title
;
 Three p-tert-Butylthiacalix[4]arene-Supported Cobalt Compounds Obtained
 in One Pot Involving In Situ Formation of N6H2 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7735
_journal_page_last               7740
_journal_paper_doi               10.1021/ic1005105
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
'[Co8(C40H44O4S4)2(N3)2(N6H2)2(CH3COO)4(CH3OH)4][OH]2(CH3OH)4'
_chemical_formula_sum            'C96 H134 Co8 N18 O26 S8'
_chemical_formula_weight         2684.13
_chemical_name_systematic        ?
_space_group_IT_number           42
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2'
_symmetry_space_group_name_H-M   'F m m 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.0575(8)
_cell_length_b                   43.5121(16)
_cell_length_c                   12.9662(5)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.32
_cell_volume                     11880.4(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker 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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21110
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         0.94
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.7280
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5552
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.080
_refine_diff_density_min         -1.640
_refine_diff_density_rms         0.338
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+32.3974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1432
_reflns_number_gt                4936
_reflns_number_total             5478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1005105_si_002_2.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4316345