Accurate Redetermination of the X-ray Structure and Electronic Bonding in Adenosylcobalamin
Lizhi Ouyang; Paul Rulis; W. Y. Ching; Giorgio Nardin; Lucio Randaccio; Inorganic Chemistry 43 (2004) 1235–1241; doi:10.1021/ic0348446

data_4310602
_publ_section_title
;
 Accurate Redetermination of the X-ray Structure and Electronic Bonding in
 Adenosylcobalamin
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1235
_journal_page_last               1241
_journal_paper_doi               10.1021/ic0348446
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety
'(C72 H100 Co N18 O17 P), 1.25(C2 H6 O), 8.25(H2 O)'
_chemical_formula_sum            'C75.75 H124 Co N18 O26.5 P'
_chemical_formula_weight         1800.83
_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                   15.194(15)
_cell_length_b                   21.32(2)
_cell_length_c                   27.55(3)
_cell_measurement_reflns_used    'three frames with I>20sigma(I)'
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      'not available'
_cell_measurement_theta_min      'not available'
_cell_volume                     8924(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'MAR 345'
_diffrn_measurement_method       '60 frames rotation 3\% phi'
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'Electra synchrotron - Trieste, Italy'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.73733
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            20226
_diffrn_reflns_theta_full        28.21
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         3.18
_diffrn_standards_decay_%        'not available'
_diffrn_standards_interval_time  'not available'
_diffrn_standards_number         'not used'
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  none
_exptl_absorpt_correction_T_min  none
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             3834
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.623
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         19149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          2.329
_refine_ls_shift/su_mean         0.094
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1357P)^2^+11.4568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1869
_refine_ls_wR_factor_ref         0.1877
_reflns_number_gt                18905
_reflns_number_total             19149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0348446si20030717_042220.cif
_cod_data_source_block           adocbl
_cod_original_cell_volume        8923(16)
_cod_original_formula_sum        'C75.75 H124 Co N18 O26.50 P'
_cod_database_code               4310602