Pentafluoropropenyl Complexes of Mercury, Germanium, Tin, and Lead Derived from (Z)-CFH═CFCF3and Their Use as Transfer Reagents
Brisdon, Alan K.; Pritchard, Robin G.; Thomas, Anthony; Organometallics 31 (2012) 1341–; doi:10.1021/om2009843

data_4067994
_publ_section_title
;
 Pentafluoropropenyl Complexes of Mercury, Germanium, Tin, and Lead
 Derived from (Z)-CFH&#x2550;CFCF3and Their Use as Transfer Reagents
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1341
_journal_paper_doi               10.1021/om2009843
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C21 H15 F5 Ge'
_chemical_formula_sum            'C21 H15 F5 Ge'
_chemical_formula_weight         434.82
_chemical_name_systematic
;
 pentafluoropropenyltriphenylgermanium
;
_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      2.3
_audit_creation_date             2009-08-06T17:19:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                109.3560(10)
_cell_angle_beta                 95.807(2)
_cell_angle_gamma                115.144(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6608(3)
_cell_length_b                   10.2660(3)
_cell_length_c                   11.7404(4)
_cell_measurement_reflns_used    4335
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_measurement_wavelength     0.71073
_cell_volume                     953.72(6)
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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      0.155713E-1
_diffrn_orient_matrix_UB_12      -0.58437E-2
_diffrn_orient_matrix_UB_13      -0.841181E-1
_diffrn_orient_matrix_UB_21      0.117863
_diffrn_orient_matrix_UB_22      0.667329E-1
_diffrn_orient_matrix_UB_23      0.392936E-1
_diffrn_orient_matrix_UB_31      0.90698E-2
_diffrn_orient_matrix_UB_32      -0.975251E-1
_diffrn_orient_matrix_UB_33      -0.155542E-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  0.065
_diffrn_reflns_av_unetI/netI     0.0454
_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       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18042
_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        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         3.5
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.654
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.6922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.784
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+2.8525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1578
_reflns_number_gt                2929
_reflns_number_total             3726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2009843_si_002.cif
_cod_data_source_block           Ph3Gepfp
_cod_original_cell_volume        953.72(5)
_cod_database_code               4067994