Crystal Chemistry of Cobalamins. Structural Characterization of the Co-S Bond in Cobalamins
Lucio Randaccio; Silvano Geremia; Giorgio Nardin; Miroslav Šlouf; Ivana Srnova; Inorganic Chemistry 38 (1999) 4087–4092; doi:10.1021/ic9903376

data_4322241
_publ_section_title
;
 Crystal Chemistry of Cobalamins. Structural Characterization of the Co-S
 Bond in Cobalamins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4087
_journal_page_last               4092
_journal_paper_doi               10.1021/ic9903376
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C63 H112.8 Cl Co N15 O24.4 P S'
_chemical_formula_weight         1628.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   15.699(14)
_cell_length_b                   22.32(2)
_cell_length_c                   24.80(7)
_cell_measurement_temperature    100(2)
_cell_volume                     8690(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     1.00000
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7715
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         5.75
_exptl_absorpt_coefficient_mu    2.870
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3464
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.092(16)
_refine_ls_extinction_coef       0.0139(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.580
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         7388
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.601
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.1129
_refine_ls_shift/su_max          2.005
_refine_ls_shift/su_mean         0.067
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3183
_refine_ls_wR_factor_ref         0.3265
_reflns_number_gt                7080
_reflns_number_total             7388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9903376_2.cif
_cod_data_source_block           '[(NH2)2CSCbl]Cl.nH2O'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        8693(27)
_cod_original_formula_sum        'C63 H112.8 Cl Co N15 O24.40 P S'
_cod_database_code               4322241