Characterization of Chlorovinylcobalamin, A Putative Intermediate in Reductive Degradation of Chlorinated Ethylenes
Kevin M. McCauley; Scott R. Wilson; Wilfred A. van der Donk; Journal of the American Chemical Society 125 (2003) 4410–4411; doi:10.1021/ja029692c

data_4113655
_publ_contact_author
; 
Wilfred A. van der Donk 
Department of Chemistry 
University of Illinois at Urbana-Champaign 
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       vddonk@uiuc.edu
_publ_contact_author_fax         '1  217 244 8024'
_publ_contact_author_phone       '1  217 244 5360'
_publ_section_title
;
 Characterization of Chlorovinylcobalamin, A Putative Intermediate in
 Reductive Degradation of Chlorinated Ethylenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4410
_journal_page_last               4411
_journal_paper_doi               10.1021/ja029692c
_journal_volume                  125
_journal_year                    2003
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C64 H90 Cl Co N13 O14 P, 17(H2 O)'
_chemical_formula_sum            'C64 H124 Cl Co N13 O31 P'
_chemical_formula_weight         1694.09
_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
_audit_update_record
; 
2003-02-13   text and data added, srw 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   29.486(4)
_cell_length_b                   29.833(4)
_cell_length_c                   37.579(5)
_cell_measurement_reflns_used    1021
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      50.8
_cell_measurement_theta_min      3.3
_cell_volume                     33057(8)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.10 (Bruker, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL V6.10 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.10 (Bruker, 2001)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Bruker Proteum/M 6000 D8'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_id  p44ofsam
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            183152
_diffrn_reflns_theta_full        58.92
_diffrn_reflns_theta_max         58.92
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  856
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.857
_exptl_absorpt_correction_T_max  0.7757
_exptl_absorpt_correction_T_min  0.4976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       prism
_exptl_crystal_F_000             14448
_exptl_crystal_id                p44ofsam
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.2 mm cryo-loop (Hampton Research) with the (1 0 -1) scattering planes 
roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.182
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.071(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4224
_refine_ls_number_reflns         46499
_refine_ls_number_restraints     6140
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.1012
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2744
_refine_ls_wR_factor_ref         0.2901
_reflns_number_gt                34988
_reflns_number_total             46499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029692csi20030220_015537.cif
_cod_data_source_block           p44ofsam
_cod_original_cell_volume        33057(7)
_cod_original_sg_symbol_Hall     'P 2ac 2ab '
_cod_database_code               4113655