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_4318457
_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         'C24 H24 F2 Ge1'
_chemical_formula_structural     'C24 H24 F2 GE1'
_chemical_formula_sum            'C24 H24 F2 Ge'
_chemical_formula_weight         423.02
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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             2001-11-20T07:20:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.7970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4276(2)
_cell_length_b                   11.4998(2)
_cell_length_c                   32.0449(5)
_cell_measurement_reflns_used    62938
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     4201.94(12)
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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      0.282686E-1
_diffrn_orient_matrix_UB_12      -0.76856E-2
_diffrn_orient_matrix_UB_13      -0.287408E-1
_diffrn_orient_matrix_UB_21      0.726528E-1
_diffrn_orient_matrix_UB_22      -0.39593E-1
_diffrn_orient_matrix_UB_23      0.119065E-1
_diffrn_orient_matrix_UB_31      -0.401715E-1
_diffrn_orient_matrix_UB_32      -0.770392E-1
_diffrn_orient_matrix_UB_33      -0.32126E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            24763
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.55
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.48
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colouress
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         9427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0573P)^2^+0.5962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                6634
_reflns_number_total             9427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025593o_s1_5.cif
_cod_data_source_block           ph3gecfcfbu
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4318457