Selectfluor-Mediated Dialkoxylation of Tungsten η2-Pyridinium Complexes
Kosturko, George W.; Harrison, Daniel P.; Sabat, Michal; Myers, William H.; Harman, W. Dean; Organometallics 28 (2009) 387–389; doi:10.1021/om801068u

data_4063498
_publ_section_title
;
 Selectfluor-Mediated Dialkoxylation of Tungsten \h2-Pyridinium Complexes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              387
_journal_page_last               389
_journal_paper_doi               10.1021/om801068u
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C22 H33 B F3 N8 O7 P S W'
_chemical_formula_weight         836.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.266(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.942(3)
_cell_length_b                   9.892(3)
_cell_length_c                   28.897(9)
_cell_measurement_reflns_used    6868
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.527
_cell_measurement_theta_min      2.801
_cell_volume                     3077.7(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            40053
_diffrn_reflns_theta_full        32.56
_diffrn_reflns_theta_max         32.56
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    3.946
_exptl_absorpt_correction_T_max  0.801926
_exptl_absorpt_correction_T_min  0.508729
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.802
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         11101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0695
_reflns_number_gt                8579
_reflns_number_total             11101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801068u_si_003.cif
_cod_data_source_block           C22H33BF3N8O7PSW
_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 1673 2011-04-08 12:14:43Z adriana 
;
_cod_original_cell_volume        3077.9(17)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4063498