Synthetic Access to a Hydrocarbon-Soluble Trifluorinated Ge(II) Compound and its Sn(II) Congener.
Samuel, Prinson P.; Li, Yan; Roesky, Herbert W.; Chevelkov, Veniamin; Lange, Adam; Burkhardt, Anja; Dittrich, Birger; Journal of the American Chemical Society 136 (2014) 1292–1295; doi:10.1021/ja412151e

data_4120478
_publ_section_title
;
 Synthetic Access to a Hydrocarbon-Soluble Trifluorinated Ge(II) Compound
 and its Sn(II) Congener.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1292
_journal_page_last               1295
_journal_paper_doi               10.1021/ja412151e
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C15 H25 N2, F3 Ge'
_chemical_formula_sum            'C15 H25 F3 Ge N2'
_chemical_formula_weight         362.98
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3477(11)
_cell_length_b                   10.5608(12)
_cell_length_c                   17.8086(19)
_cell_measurement_reflns_used    4869
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.242
_cell_volume                     1758.1(3)
_computing_cell_refinement       'SAINT V8.32B'
_computing_data_collection       'APEX2 v2012.2 (Bruker AXS, 2012)'
_computing_data_reduction        'SAINT V8.32B'
_computing_molecular_graphics    'Shelxle (Huebschle, 2013)'
_computing_publication_material  'enCIFer 1.4, CCDC, 2011'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -2.2569629e-03
_diffrn_orient_matrix_UB_12      -7.5388779e-03
_diffrn_orient_matrix_UB_13      -5.5961803e-02
_diffrn_orient_matrix_UB_21      -1.0682275e-01
_diffrn_orient_matrix_UB_22      -4.5135273e-03
_diffrn_orient_matrix_UB_23      1.4008259e-03
_diffrn_orient_matrix_UB_31      -5.2944073e-03
_diffrn_orient_matrix_UB_32      9.4281070e-02
_diffrn_orient_matrix_UB_33      -4.4077407e-03
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15229
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.546
_diffrn_reflns_theta_min         2.242
_diffrn_source                   'INCOATEC Mo Microsource'
_exptl_absorpt_coefficient_mu    1.766
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6604
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2008/2, multi-scan. (G. M. Sheldrick, 2008)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.98
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.319(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4054
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+0.0367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.752
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3642
_reflns_number_total             4054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja412151e_si_002.cif
_cod_data_source_block           ps301
_cod_database_code               4120478
_shelxl_version_number           2013-4
_shelx_res_checksum              82062
_shelx_hkl_checksum              90896