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_4302674
_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            'C64 H95 Co N14 O14 P'
_chemical_formula_weight         1374.44
_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                   16.0000(10)
_cell_length_b                   21.0200(10)
_cell_length_c                   24.5400(10)
_cell_measurement_temperature    293(2)
_cell_volume                     8253.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.763
_diffrn_measured_fraction_theta_max 0.763
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.78468
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            131855
_diffrn_reflns_theta_full        33.54
_diffrn_reflns_theta_max         33.54
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.288
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2924
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.070(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1037
_refine_ls_number_reflns         18317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          6.860
_refine_ls_shift/su_mean         0.031
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1126P)^2^+10.4173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                18291
_reflns_number_total             18317
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4302672
_cod_data_source_file            ic900590p_si_003_1.cif
_cod_data_source_block           ethc_mk
_cod_database_code               4302674