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_4318453
_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 Ge'
_chemical_formula_structural     'C20 H15 F3 GE'
_chemical_formula_sum            'C20 H15 F3 Ge'
_chemical_formula_weight         384.91
_chemical_name_systematic
;
 (trifluorovinyl)triphenylgermanium
;
_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             2001-06-28T15:32:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                103.05(4)
_cell_angle_beta                 95.43(3)
_cell_angle_gamma                108.91(2)
_cell_formula_units_Z            4
_cell_length_a                   10.087(2)
_cell_length_b                   10.338(5)
_cell_length_c                   18.704(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      13.16
_cell_measurement_theta_min      8.08
_cell_measurement_wavelength     0.71073
_cell_volume                     1767.5(13)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.8156E-2
_diffrn_orient_matrix_UB_12      0.61739E-1
_diffrn_orient_matrix_UB_13      -0.34782E-1
_diffrn_orient_matrix_UB_21      0.10569
_diffrn_orient_matrix_UB_22      0.25724E-1
_diffrn_orient_matrix_UB_23      0.8826E-2
_diffrn_orient_matrix_UB_31      -0.10148E-1
_diffrn_orient_matrix_UB_32      -0.82803E-1
_diffrn_orient_matrix_UB_33      -0.42779E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6534
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.14
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.759
_exptl_absorpt_correction_T_max  0.5873
_exptl_absorpt_correction_T_min  0.1595
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   3
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6147
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1488
_refine_ls_R_factor_gt           0.0648
_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^)+(0.0862P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.139
_refine_ls_wR_factor_ref         0.1716
_reflns_number_gt                3254
_reflns_number_total             6147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025593o_s1_1.cif
_cod_data_source_block           ph3gepfv
_cod_original_cell_volume        1767.4(12)
_cod_database_code               4318453
_exptl_absorpt_factor_mur        0.528
_exptl_absorpt_correction_t_ave  0.4071
_diffrn_standards_decay_corr_max 1.059
_diffrn_standards_decay_corr_min 0.985