Cis Effects in the Cobalt Corrins. 1. Crystal Structures of 10-Chloroaquacobalamin Perchlorate, 10-Chlorocyanocobalamin, and 10-Chloromethylcobalamin
Kenneth L. Brown; Shifa Cheng; Xiang Zou; Jeffrey D. Zubkowski; Edward J. Valente; Leanne Knapton; Helder M. Marques; Inorganic Chemistry 36 (1997) 3666–3675; doi:10.1021/ic9615077

data_4323527
_publ_section_title
;
 Cis Effects in the Cobalt Corrins. 1. Crystal Structures of
 10-Chloroaquacobalamin Perchlorate, 10-Chlorocyanocobalamin, and
 10-Chloromethylcobalamin
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3666
_journal_page_last               3675
_journal_paper_doi               10.1021/ic9615077
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        'Brown synthesis'
_chemical_formula_sum            'C63 H134 Cl Co N11 O34 P'
_chemical_formula_weight         1715.18
_chemical_name_common            'Methyl 10-chlorocobalamin acetone 20hydrate'
_chemical_name_systematic        'Methyl 10-chlorocobalamin acetone 20hydrate'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.041(14)
_cell_length_b                   22.132(21)
_cell_length_c                   26.750(35)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      20.
_cell_measurement_theta_min      12.
_cell_volume                     9497(17)
_computing_cell_refinement       'P3 (Siemens Analytical X-ray)'
_computing_data_collection       'P3 (Siemens Analytical X-ray)'
_computing_data_reduction        'XDISK (Siemens Analytical X-ray)'
_computing_molecular_graphics    'XP (Siemens Analytical X-ray)'
_computing_publication_material  SHELXL/CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device       'scintillation counter'
_diffrn_measurement_method       'omega 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  0.3130
_diffrn_reflns_av_sigmaI/netI    0.2917
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6810
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  1hr
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  NA
_exptl_absorpt_correction_T_min  NA
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            wine-red
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    NA
_exptl_crystal_description       'elongated prism'
_exptl_crystal_F_000             3688
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.661
_refine_ls_goodness_of_fit_obs   1.277
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1011
_refine_ls_number_reflns         6791
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      0.723
_refine_ls_restrained_S_obs      1.247
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_obs          0.0554
_refine_ls_shift/esd_max         0.677
_refine_ls_shift/esd_mean        0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1347
_refine_ls_wR_factor_obs         0.1072
_reflns_number_observed          2145
_reflns_number_total             6792
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9615077_3.cif
_cod_data_source_block           METHYL_10-CHLOROCOBALAMIN_ACETONE_HYDRATE
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NA' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0496P)^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^)+(0.0496P)^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        9496.8(174)
_cod_database_code               4323527