Structure and Reversible Pyran Formation in Molybdenum Pyranopterin Dithiolene Models of the Molybdenum Cofactor
Benjamin R. Williams; Yichun Fu; Glenn P. A. Yap; Sharon J. Nieter Burgmayer; Journal of the American Chemical Society 134 (2012) 19584–19587; doi:10.1021/ja310018e

data_4118959
_publ_section_title
;
 Structure and Reversible Pyran Formation in Molybdenum Pyranopterin
 Dithiolene Models of the Molybdenum Cofactor
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19584
_journal_page_last               19587
_journal_paper_doi               10.1021/ja310018e
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C31 H41 B Mo N11 O4 S2, 3.5(C2 H4 Cl2)'
_chemical_formula_sum            'C38 H55 B Cl7 Mo N11 O4 S2'
_chemical_formula_weight         1148.95
_chemical_name_common            MoTp*(O)(S2BMOPP
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 97.583(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.1966(5)
_cell_length_b                   17.0102(5)
_cell_length_c                   42.0911(16)
_cell_measurement_reflns_used    3564
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      18.97
_cell_measurement_theta_min      2.25
_cell_volume                     10075.6(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1553
_diffrn_reflns_av_sigmaI/netI    0.1453
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            120279
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.9679
_exptl_absorpt_correction_T_min  0.8633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       plate
_exptl_crystal_F_000             4720
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
PLATON: Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
        Spek, A.L. (2009). Acta Cryst. D65, 148-155.
Void space analysis consistent with 28 molecules of
dichloroethane solvent per unit cell.
;
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         20602
_refine_ls_number_restraints     936
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0144P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0951
_reflns_number_gt                9976
_reflns_number_total             20602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja310018e_si_001_2.cif
_cod_data_source_block           burg001-sr
_cod_database_code               4118959