Synthesis and structural characterisation of polynuclear cobalt complexes with partially-deprotonated Bis-tris.
Ferguson, Alan; Parkin, Andrew; Murrie, Mark; Dalton transactions (Cambridge, England : 2003)  (2006) 3627–3628; doi:10.1039/b603622h

data_7007321
_publ_section_title
;
 Synthesis and structural characterisation of polynuclear cobalt
 complexes with partially-deprotonated Bis-tris.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3627
_journal_page_last               3628
_journal_paper_doi               10.1039/b603622h
_journal_year                    2006
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C34 H70 Co5 N4 O22'
_chemical_formula_sum            'C34 H70 Co5 N4 O22'
_chemical_formula_weight         1181.61
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-05-20
_audit_creation_method           CRYSTALS_ver_12.83
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2070(7)
_cell_length_b                   13.2070(7)
_cell_length_c                   12.5890(8)
_cell_measurement_reflns_used    301848
_cell_measurement_temperature    100
_cell_measurement_theta_max      28
_cell_measurement_theta_min      0
_cell_volume                     2195.8(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.087
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2538
_diffrn_reflns_theta_full        27.550
_diffrn_reflns_theta_max         27.550
_diffrn_reflns_theta_min         2.235
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.938
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_description       block
_exptl_crystal_F_000             1226
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.56
_refine_diff_density_min         -0.53
_refine_ls_abs_structure_details 'Flack (1983), 1104 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2538
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.003078
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 0.00P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1134
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1134
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                1874
_reflns_number_total             2538
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.638(2)
_oxford_structure_analysis_title 'CRYSTALS_cif in P -4 21 c'
_cod_data_source_file            b603622h.txt
_cod_data_source_block           2
_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_sg_symbol_H-M      'P -4 21 c '
_cod_database_code               7007321