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_4323525
_publ_section_title
;
 Cis Effects in the Cobalt Corrins. 1. Crystal Structures of
 10-Chloroaquacobalamin Perchlorate, 10-Chlorocyanocobalamin, and
 10-Chloromethylcobalamin
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_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            'C68 H123 Cl2 Co N13 O32 P'
_chemical_formula_weight         1795.59
_chemical_name_common            'Aqua 10-chlorocobalamin perchlorate solvate'
_chemical_name_systematic        'Aqua 10-chlorocobalamin perchlorate solvate'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 93.05(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.922(4)
_cell_length_b                   26.592(10)
_cell_length_c                   13.511(5)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      23.5
_cell_measurement_theta_min      12.5
_cell_volume                     4277(3)
_computing_cell_refinement       'P3 Siemens Analytical X-ray'
_computing_data_collection       'P3 Siemens Analytical X-ray'
_computing_data_reduction        'P3 Siemens Analytical X-ray'
_computing_molecular_graphics    'XP Siemens Analytical X-ray'
_computing_publication_material  'SHELXL (Sheldrick)'
_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         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.1313
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11296
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  'variable, 1 - 1.5 hrs'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  NA
_exptl_absorpt_correction_T_min  NA
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       'Thin block'
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(14)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.736
_refine_ls_goodness_of_fit_obs   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         10534
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      0.833
_refine_ls_restrained_S_obs      0.974
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_obs          0.0426
_refine_ls_shift/esd_max         1.200
_refine_ls_shift/esd_mean        0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1050
_refine_ls_wR_factor_obs         0.0887
_reflns_number_observed          5987
_reflns_number_total             10535
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9615077_1.cif
_cod_data_source_block           10-CHLORO_AQUACOBALAMIN_PERCHLORATE_HYDRATE
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0362P)^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^)+(0.0362P)^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 
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_cod_original_cell_volume        4277.3(27)
_cod_database_code               4323525