Trans and Cis Effects of Axial Fluoroalkyl Ligands in Vitamin B12 Analogues: Relationship between Alkyl- and Fluoroalkyl-Cobalamins
Lucio Randaccio; Giovanna Brancatelli; Nicola Demitri; Renata Dreos; Neal Hickey; Patrizia Siega; Silvano Geremia; Inorganic Chemistry 52 (2013) 13392–13401; doi:10.1021/ic401715e

data_4336807
_publ_section_title
;
 Trans and Cis Effects of Axial Fluoroalkyl Ligands in Vitamin B12
 Analogues: Relationship between Alkyl- and Fluoroalkyl-Cobalamins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13392
_journal_page_last               13401
_journal_paper_doi               10.1021/ic401715e
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C62.93 H88 N13 O14 P Co F2.79 I0.07, 1.5(C3 H6 O), 8.35 (O)'
_chemical_formula_sum            'C67.46 H97 Co F2.79 I0.07 N13 O23.85 P'
_chemical_formula_weight         1623.49
_chemical_name_systematic
;
 trifluoromethyl-cobalamine
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5600(3)
_cell_length_b                   22.5900(8)
_cell_length_c                   24.9700(7)
_cell_measurement_temperature    100(2)
_cell_volume                     8777.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.884
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_wavelength     0.7
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14414
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         10.09
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  1.4828
_exptl_absorpt_correction_T_min  0.5533
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
        cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_F_000             3501
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.035(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1034
_refine_ls_number_reflns         14414
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.091
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1041P)^2^+6.8409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.1876
_reflns_number_gt                13145
_reflns_number_total             14414
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic401715e_si_002.cif
_cod_data_source_block           CF3Cbl
_cod_database_code               4336807