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_4118958
_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_absolute_configuration ad
_chemical_formula_sum            'C45 H67 B Cl18 Mo N12 O4 S2'
_chemical_formula_weight         1649.08
_chemical_name_common            TEA[MoTp*(O)(S2BMOPP)]
_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
;
2012-10-04 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7048(7)
_cell_length_b                   18.8549(10)
_cell_length_c                   29.2118(14)
_cell_measurement_reflns_used    3650
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      34.17
_cell_measurement_theta_min      2.79
_cell_volume                     7548.4(7)
_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 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_sigmaI/netI    0.1227
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16447
_diffrn_reflns_theta_full        48.45
_diffrn_reflns_theta_max         48.45
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    8.176
_exptl_absorpt_correction_T_max  0.4585
_exptl_absorpt_correction_T_min  0.3815
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       prism
_exptl_crystal_F_000             3352
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;

PLATON Reference : 
 Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
 Spek, A.L. (2009). Acta Cryst. D65, 148-155.

Void space analysis suggests 24 CHCl3 molecules cocrystallized 
in the unit cell. Initial solutions show only 8 solvent molecules
per unit cell.
;
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.073(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         6462
_refine_ls_number_restraints     580
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1334
_reflns_number_gt                3595
_reflns_number_total             6462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja310018e_si_001_1.cif
_cod_data_source_block           burg002s-sr
_cod_database_code               4118958