A tetranuclear cobalt(III) cluster with 2-(hydroxymethyl)pyridine ligands
Wang, Fang-Ming; Lu, Chang-Sheng; Li, Yi-Zhi; Meng, Qing-Jin; Acta Crystallographica Section E 66 (2010) m594–; doi:10.1107/S1600536810015369

data_2225793
_publ_section_title
;
 A tetranuclear cobalt(III) cluster with 2-(hydroxymethyl)pyridine
 ligands
;
_journal_coeditor_code           BX2274
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m594
_journal_paper_doi               10.1107/S1600536810015369
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Co4 Br4 (C6 H6 N O)4 (C H4 O)4] Br4, 4C6 H7 N O4, 2H2 O'
_chemical_formula_moiety
'C28 H40 Br4 Co4 N4 O8 4+, 4(Br -), 4(C6 H7 N O), 2(H2 O)'
_chemical_formula_sum            'C52 H72 Br8 Co4 N8 O14'
_chemical_formula_weight         1908.10
_chemical_name_systematic
;
tetrakis[\m~3~-(2-pyridyl)methanolato]tetrakis[bromido(methanol)cobalt(III)]
tetrabromide 2-(hydroxymethyl)pyridine tetrasolvate dihydrate
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_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                   16.5302(6)
_cell_length_b                   16.5302(6)
_cell_length_c                   29.875(2)
_cell_measurement_reflns_used    4154
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      23.11
_cell_measurement_theta_min      2.21
_cell_volume                     8163.3(7)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            21461
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    4.767
_exptl_absorpt_correction_T_max  0.350
_exptl_absorpt_correction_T_min  0.265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.564
_refine_ls_abs_structure_details 'Flack (1983), 1822 Friedel pairs'
_refine_ls_abs_structure_Flack   0.025(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0635P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                3180
_reflns_number_total             4018
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bx2274.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        8163.3(8)
_cod_original_sg_symbol_H-M      'I -42 d'
_cod_database_code               2225793
_cod_database_fobs_code          2225793