Synthesis and Characterization of Chlorinated Alkenylcobaloximes To Probe the Mechanism of Vitamin B12-Catalyzed Dechlorination of Priority Pollutants
Kevin M. McCauley; Scott R. Wilson; Wilfred A. van der Donk; Inorganic Chemistry 41 (2002) 393–404; doi:10.1021/ic011023x

data_4317467
_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
;
 Synthesis and Characterization of Chlorinated Alkenylcobaloximes To Probe
 the Mechanism of Vitamin B12-Catalyzed Dechlorination of Priority
 Pollutants
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              393
_journal_page_last               404
_journal_paper_doi               10.1021/ic011023x
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '3(C15 H21 Cl Co N5 O4), C H2 Cl2'
_chemical_formula_sum            'C15.33 H21.67 Cl1.67 Co N5 O4'
_chemical_formula_weight         458.06
_chemical_name_common            Co(dmgH)2(py)(CCl=CH2)
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
?
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.6100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   8.8489(8)
_cell_length_b                   39.436(4)
_cell_length_c                   16.9814(16)
_cell_measurement_reflns_used    4131
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4
_cell_volume                     5804.7(10)
_computing_cell_refinement       'SAINT V5 (Bruker, 1998)'
_computing_data_collection       'SMART V5 (Bruker, 1998)'
_computing_data_reduction        'SAINT V5 (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL V5 (Bruker, 1998)'
_computing_publication_material  'CIFTAB (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL V5 (Bruker, 1998)'
_computing_structure_solution    'SHELXTL V5 (Bruker, 1998)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1901
_diffrn_reflns_av_sigmaI/netI    0.2304
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34618
_diffrn_reflns_theta_full        23.02
_diffrn_reflns_theta_max         23.02
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        4.8
_diffrn_standards_interval_time  730
_diffrn_standards_number         136
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  0.9768
_exptl_absorpt_correction_T_min  0.8057
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Bruker, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       needle
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         8103
_refine_ls_number_restraints     471
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.1786
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0080P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                3640
_reflns_number_total             8103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011023x_3.cif
_cod_data_source_block           p05le
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        5804.6(9)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4317467