Sequential Tandem Addition to a Tungsten-Trifluorotoluene Complex: A Versatile Method for the Preparation of Highly Functionalized Trifluoromethylated Cyclohexenes.
Wilson, Katy B.; Myers, Jeffery T.; Nedzbala, Hannah S.; Combee, Logan A.; Sabat, Michal; Harman, W. Dean; Journal of the American Chemical Society 139 (2017) 11401–11412; doi:10.1021/jacs.7b05118

data_4131398
_publ_section_title
;
 Sequential Tandem Addition to a Tungsten-Trifluorotoluene Complex: A
 Versatile Method for the Preparation of Highly Functionalized
 Trifluoromethylated Cyclohexenes.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11401
_journal_page_last               11412
_journal_paper_doi               10.1021/jacs.7b05118
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C25 H37 B F3 N8 O3 P W'
_chemical_formula_weight         780.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.5240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3421(9)
_cell_length_b                   16.1680(9)
_cell_length_c                   23.4046(12)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      31.39
_cell_measurement_theta_min      3.72
_cell_volume                     6155.2(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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            120729
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.625
_diffrn_reflns_theta_min         3.430
_exptl_absorpt_coefficient_mu    3.865
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6397
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         19833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+2.8730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17498
_reflns_number_total             19833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b05118_si_003.cif
_cod_data_source_block           C25H37BF3N8O3PW
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4131398
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.353
_shelx_estimated_absorpt_t_max   0.457
_shelx_res_checksum              72251
_shelx_hkl_checksum              94652