Preparation and X-ray Analysis of Crystals of Azido- and Chlorocobalamin Containing LiCl: A Structural Model for the Interactions of the Corrin Ring with Ionic Species
Lucio Randaccio; Michela Furlan; Silvano Geremia; Miroslav Slouf; Inorganic Chemistry 37 (1998) 5390–5393; doi:10.1021/ic980181u

data_4323050
_publ_section_title
;
 Preparation and X-ray Analysis of Crystals of Azido- and Chlorocobalamin
 Containing LiCl: A Structural Model for the Interactions of the Corrin
 Ring with Ionic Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5390
_journal_page_last               5393
_journal_paper_doi               10.1021/ic980181u
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'N3-Cbl . 2LiCl . 9.3H2O'
_chemical_formula_sum            'C62 H106.6 Cl2 Co Li2 N16 O23.3 P'
_chemical_formula_weight         1623.71
_chemical_name_common            Azidocobalamine
_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                   15.4340(10)
_cell_length_b                   22.6790(10)
_cell_length_c                   23.4500(10)
_cell_measurement_reflns_used    'all - Denzo'
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.15
_cell_volume                     8208.1(7)
_computing_cell_refinement       Scalepack
_computing_data_collection       MAR345
_computing_data_reduction        DENZO
_computing_molecular_graphics    PLATON
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'isomorphous replacement'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'image plate mar345'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  'silicone 110'
_diffrn_radiation_source         wiggler
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80000
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11828
_diffrn_reflns_theta_full        27.03
_diffrn_reflns_theta_max         27.03
_diffrn_reflns_theta_min         4.64
_diffrn_standards_decay_%        'no standards'
_diffrn_standards_interval_count 'no standards'
_diffrn_standards_interval_time  'no standards'
_diffrn_standards_number         'no standards'
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  'not done'
_exptl_absorpt_correction_T_min  'not done'
_exptl_absorpt_correction_type   'not done'
_exptl_crystal_colour            scarlet
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisma
_exptl_crystal_F_000             3436
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1016
_refine_ls_number_reflns         11828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          8.863
_refine_ls_shift/su_mean         0.060
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+10.3232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1457
_reflns_number_gt                11683
_reflns_number_total             11828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980181u_2.cif
_cod_data_source_block           b12n3lt
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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^)+(0.0936P)^2^+10.3232P] 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^)+(0.0936P)^2^+10.3232P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C62 H106.60 Cl2 Co Li2 N16 O23.30 P'
_cod_database_code               4323050