Neutral Pentacoordinate Group 14 Compounds with β-Diketonato ligands
Bombicz, Petra; Kovács, Ilona; Nyulászi, László; Szieberth, Dénes; Terleczky, Péter; Organometallics 29 (2010) 1100–; doi:10.1021/om900779s

data_4067290
_publ_section_title
;
 Neutral Pentacoordinate Group 14 Compounds with \b-Diketonato ligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1100
_journal_paper_doi               10.1021/om900779s
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C18 H11 F9 Ge O2'
_chemical_formula_weight         502.86
_chemical_name_systematic
; 
4,6-diphenyl-2,2,2-tris(trifluoromethyl)-2H,4H-1,3,2-dioxagermin-2-ium-4-ide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             07-06-22
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.02(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.612(4)
_cell_length_b                   14.042(3)
_cell_length_c                   13.579(3)
_cell_measurement_reflns_used    19570
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.8470
_cell_measurement_theta_min      2.9612
_cell_volume                     3611.8(14)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device
;
RAXIS conversion
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       RX
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1146
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            84243
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_diffrn_source_current           40.0000
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_T_max  0.6619
_exptl_absorpt_correction_T_min  0.3456
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   numerical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.581
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.0005(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         6351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1166P)^2^+2.5390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1695
_refine_ls_wR_factor_ref         0.1755
_reflns_number_gt                6021
_reflns_number_total             6353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900779s_si_002.cif
_cod_data_source_block           ki58Ge
_cod_original_cell_volume        3611.8(12)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4067290