Friedel‒Crafts Ring-Coupling Reactions Promoted by Tungsten Dearomatization Agent
Pienkos, Jared A.; Zottig, Victor E.; Iovan, Diana A.; Li, Mengxun; Harrison, Daniel P.; Sabat, Michal; Salomon, Rebecca J.; Strausberg, Laura; Teran, Victor A.; Myers, William H.; Harman, W. Dean; Organometallics 32 (2013) 691–; doi:10.1021/om3012008

data_4080026
_publ_section_title
;
 Friedel--Crafts Ring-Coupling Reactions Promoted by Tungsten
 Dearomatization Agent
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              691
_journal_paper_doi               10.1021/om3012008
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C30 H42 B Cl F3 N8 O7 P S W'
_chemical_formula_weight         976.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 127.331(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.7570(3)
_cell_length_b                   16.5592(2)
_cell_length_c                   14.7772(2)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      36.33
_cell_measurement_theta_min      2.46
_cell_volume                     3844.14(10)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21323
_diffrn_reflns_theta_full        36.33
_diffrn_reflns_theta_max         36.33
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    3.240
_exptl_absorpt_correction_T_max  0.5228
_exptl_absorpt_correction_T_min  0.3647
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.847
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(4)
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         9466
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0204
_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^)+(0.1000P)^2^+0.2500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0597
_reflns_number_gt                9186
_reflns_number_total             9466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3012008_si_002.cif
_cod_data_source_block           C30H42BF3N8O7PClW
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3844.19(9)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4080026