Spectroscopic and Structural Assignment of the Absolute Stereochemistry in a Series of 1,2-Difluorovinyl Organometalloids. The First Crystallographic Characterization and Structural Series of Group 14 Fluorovinyl Compounds
Alan K. Brisdon; Ian R. Crossley; Robin G. Pritchard; John E. Warren; Inorganic Chemistry 41 (2002) 4748–4755; doi:10.1021/ic025593o

data_4318454
_publ_section_title
;
 Spectroscopic and Structural Assignment of the Absolute Stereochemistry
 in a Series of 1,2-Difluorovinyl Organometalloids. The First
 Crystallographic Characterization and Structural Series of Group 14
 Fluorovinyl Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4748
_journal_page_last               4755
_journal_paper_doi               10.1021/ic025593o
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C20 H15 F3 Sn1'
_chemical_formula_sum            'C20 H15 F3 Sn'
_chemical_formula_weight         431.01
_chemical_melting_point          346
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-01-10T14:46:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.020(4)
_cell_angle_beta                 85.893(4)
_cell_angle_gamma                87.843(3)
_cell_formula_units_Z            4
_cell_length_a                   9.6807(6)
_cell_length_b                   9.9819(8)
_cell_length_c                   18.2114(14)
_cell_measurement_reflns_used    5078
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     1754.0(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.158271E-1
_diffrn_orient_matrix_UB_12      0.718862E-1
_diffrn_orient_matrix_UB_13      0.363885E-1
_diffrn_orient_matrix_UB_21      0.94909E-1
_diffrn_orient_matrix_UB_22      0.118208E-1
_diffrn_orient_matrix_UB_23      -0.240146E-1
_diffrn_orient_matrix_UB_31      -0.38505E-1
_diffrn_orient_matrix_UB_32      0.688714E-1
_diffrn_orient_matrix_UB_33      -0.336144E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10924
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.11
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  0.8658
_exptl_absorpt_correction_T_min  0.7558
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         6.496
_refine_diff_density_min         -1.879
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.087
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1423P)^2^+12.9456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2216
_refine_ls_wR_factor_ref         0.246
_reflns_number_gt                5453
_reflns_number_total             7203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025593o_s1_2.cif
_cod_data_source_block           ph3snpfv
_cod_original_formula_sum        'C20 H15 F3 Sn1'
_cod_database_code               4318454