Similarities and Differences between Cobalamins and Cobaloximes. Accurate Structural Determination of Methylcobalamin and of LiCl- and KCl-Containing Cyanocobalamins by Synchrotron Radiation
Lucio Randaccio; Michela Furlan; Silvano Geremia; Miroslav Šlouf; Ivana Srnova; Daniele Toffoli; Inorganic Chemistry 39 (2000) 3403–3413; doi:10.1021/ic0001199

data_4321144
_publ_contact_author
;
    Lucio Randaccio
    Dipartimento di Scienze Chimiche
    Universita' di Trieste
    34127 Trieste 
    Italy
;
_publ_contact_author_email       randaccio@univ.trieste.it
_publ_section_title
;
 Similarities and Differences between Cobalamins and Cobaloximes. Accurate
 Structural Determination of Methylcobalamin and of LiCl- and
 KCl-Containing Cyanocobalamins by Synchrotron Radiation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3403
_journal_page_last               3413
_journal_paper_doi               10.1021/ic0001199
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         '(Co1 C63 H91 N13 O14 P1) 18.1(H2O) '
_chemical_formula_sum            'C63 H127.2 Co N13 O32.1 P'
_chemical_formula_weight         1670.48
_chemical_name_systematic
; 
 methylcobalamin solvated
;
_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                   17.280(5)
_cell_length_b                   17.740(5)
_cell_length_c                   32.370(5)
_cell_measurement_temperature    100(2)
_cell_volume                     9923(4)
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_molecular_graphics    'ORTEP graphics'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Mar 345 Imaging Plate'
_diffrn_radiation_monochromator  'Si 110'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80000
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            15897
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_type   no
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3580
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(14)
_refine_ls_extinction_coef       0.0167(15)
_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   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         15154
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          5.345
_refine_ls_shift/su_mean         0.249
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1948P)^2^+1.8217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2312
_refine_ls_wR_factor_ref         0.2398
_reflns_number_gt                13535
_reflns_number_total             15154
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0001199_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1948P)^2^+1.8217P] 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^)+(0.1948P)^2^+1.8217P] 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        'C63 H127.20 Co N13 O32.10 P'
_cod_database_code               4321144