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_4318456
_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 H16 F2 Ge1'
_chemical_formula_structural     'C20 H16 F2 Ge1'
_chemical_formula_sum            'C20 H16 F2 Ge'
_chemical_formula_weight         366.92
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_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_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             2001-07-27T15:21:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 129.109(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2386(6)
_cell_length_b                   29.170(3)
_cell_length_c                   7.3196(6)
_cell_measurement_reflns_used    1013
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     1696.3(3)
_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, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_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      0.135874E-1
_diffrn_orient_matrix_UB_12      -0.7391E-2
_diffrn_orient_matrix_UB_13      -0.1206
_diffrn_orient_matrix_UB_21      -0.969878E-1
_diffrn_orient_matrix_UB_22      -0.217687E-1
_diffrn_orient_matrix_UB_23      -0.780146E-1
_diffrn_orient_matrix_UB_31      -0.790728E-1
_diffrn_orient_matrix_UB_32      0.254307E-1
_diffrn_orient_matrix_UB_33      -0.101831
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2206
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.821
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2206
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+3.4034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1075
_reflns_number_gt                1983
_reflns_number_total             2206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025593o_s1_4.cif
_cod_data_source_block           ph3gecfcfh
_cod_original_cell_volume        1696.3(2)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4318456