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_4120477
_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, 0.5(F6 Sn2)'
_chemical_formula_sum            'C15 H25 F3 N2 Sn'
_chemical_formula_weight         408.84
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 105.99(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.573(5)
_cell_length_b                   17.473(4)
_cell_length_c                   11.177(12)
_cell_measurement_reflns_used    8322
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      21.7
_cell_measurement_theta_min      1.93
_cell_volume                     1797(2)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'XDS (Kabsch, 2010)'
_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      120(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Microdiffractometer at P11 (PetraIII)'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6199
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9783
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        21.835
_diffrn_reflns_theta_max         21.793
_diffrn_reflns_theta_min         1.930
_diffrn_source                   'monochromated X-rays on beamline P11'
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6320
_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    1.510
_exptl_crystal_description       needle
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0318(17)
_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   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3192
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+1.5365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2973
_reflns_number_total             3192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja412151e_si_003.cif
_cod_data_source_block           ps302b
_cod_database_code               4120477
_shelxl_version_number           2013-4
_shelx_res_checksum              95947
_shelx_hkl_checksum              92052