Trifluoracetic Acid-Assisted Crystallization of Vitamin B12 Results in Protonation of the Phosphate Group of the Nucleotide Loop: Insight into the Influence of Crystal Packing Forces on Vitamin B12 Structures
Nadia Marino; Amy E. Rabideau; Robert P. Doyle; Inorganic Chemistry 50 (2011) 220–230; doi:10.1021/ic101810v

data_4324116
_publ_section_title
;
 Trifluoracetic Acid-Assisted Crystallization of Vitamin B12 Results in
 Protonation of the Phosphate Group of the Nucleotide Loop: Insight into
 the Influence of Crystal Packing Forces on Vitamin B12 Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              220
_journal_page_last               230
_journal_paper_doi               10.1021/ic101810v
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C63 H89 Co N14 O14 P, C2 F3 O2, 14(H2 O)'
_chemical_formula_sum            'C65 H117 Co F3 N14 O30 P'
_chemical_formula_weight         1721.63
_chemical_name_common
'hydrogenocyanocobalamin tetrafluoroacetate tetradecahydrate'
_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                   16.0692(15)
_cell_length_b                   20.818(2)
_cell_length_c                   24.081(2)
_cell_measurement_reflns_used    8830
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.33
_cell_volume                     8055.8(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20116
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3656
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983)'
_refine_ls_abs_structure_Flack   -0.004(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1120
_refine_ls_number_reflns         20116
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+2.9745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                19093
_reflns_number_total             20116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101810v_si_001.cif
_cod_data_source_block           1
_cod_database_code               4324116