High Resolution Crystal Structure of the Methylcobalamin Analogues Ethylcobalamin and Butylcobalamin by X-ray Synchrotron Diffraction
Luciana Hannibal; Clyde A. Smith; Jessica A. Smith; Armend Axhemi; Abby Miller; Sihe Wang; Nicola E. Brasch; Donald W. Jacobsen; Inorganic Chemistry 48 (2009) 6615–6622; doi:10.1021/ic900590p

data_4302677
_publ_section_title
;
High Resolution Crystal Structure of the Methylcobalamin Analogues
Ethylcobalamin and Butylcobalamin by X-ray Synchrotron Diffraction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6615
_journal_page_last               6622
_journal_paper_doi               10.1021/ic900590p
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C66 H101 Co N13 O35 P'
_chemical_formula_weight         1726.50
_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                   16.0300(10)
_cell_length_b                   20.7300(10)
_cell_length_c                   24.6200(10)
_cell_measurement_temperature    100(2)
_cell_volume                     8181.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.872
_diffrn_measured_fraction_theta_max 0.872
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_wavelength     0.78468
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            66411
_diffrn_reflns_theta_full        33.60
_diffrn_reflns_theta_max         33.60
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.336
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3640
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.095(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.769
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1136
_refine_ls_number_reflns         20414
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      0.766
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1028P)^2^+12.8608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                20171
_reflns_number_total             20414
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ic900590p_si_005.cif
_cod_data_source_block           butc_r3
_cod_database_code               4302677