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_4323526
_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            'C66 H135 Cl Co N14 O39 P'
_chemical_formula_weight         1874.23
_chemical_name_common            '10-chloro cyanocobalamin solvate'
_chemical_name_systematic        '10-Chloro cyanocobalamin solvate'
_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                   16.235(33)
_cell_length_b                   21.853(46)
_cell_length_c                   26.755(81)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      10.
_cell_volume                     9492(4)
_computing_cell_refinement       'P3 (Siemens Analytical XRay Inc.)'
_computing_data_collection       'P3 (Siemens Analytical XRay Inc.)'
_computing_data_reduction        'XDISK (Siemens Analytical XRay Inc.)'
_computing_molecular_graphics    'XP (Siemens Analytical XRay Inc.)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device
'scintillation counter, pulse-height analysis'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.2873
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9978
_diffrn_reflns_theta_max         21.61
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  5400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.315
_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    1.311
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    NA
_exptl_crystal_description       prism
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.894
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         7699
_refine_ls_number_restraints     421
_refine_ls_restrained_S_all      0.920
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.1966
_refine_ls_R_factor_obs          0.0698
_refine_ls_shift/esd_max         1.277
_refine_ls_shift/esd_mean        0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0732
_refine_ls_wR_factor_obs         0.0504
_reflns_number_observed          3168
_reflns_number_total             7700
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9615077_2.cif
_cod_data_source_block           CYANO_10-CHLOROCOBALAMIN_SOLVATE
_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^)+(0.0000P)^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^)+(0.0000P)^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        9492.2(400)
_cod_database_code               4323526