Phosphine-Stabilized Digermavinylidene.
Krebs, Kilian M.; Hanselmann, Dominik; Schubert, Hartmut; Wurst, Kai; Scheele, Marcus; Wesemann, Lars; Journal of the American Chemical Society 141 (2019) 3424–3429; doi:10.1021/jacs.8b13645

data_4127794
_publ_section_title
;
 Phosphine-Stabilized Digermavinylidene.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3424
_journal_page_last               3429
_journal_paper_doi               10.1021/jacs.8b13645
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C60 H69 Ge2 P'
_chemical_formula_weight         966.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                83.4320(10)
_cell_angle_beta                 81.1790(10)
_cell_angle_gamma                88.2720(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5389(2)
_cell_length_b                   16.2601(4)
_cell_length_c                   16.9069(4)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.52
_cell_volume                     2574.08(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            61324
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.538
_diffrn_reflns_theta_min         1.854
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.190
_refine_diff_density_max         1.173
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         15609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+1.0573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13036
_reflns_number_total             15609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13645_si_005.cif
_cod_data_source_block           shelx
_cod_database_code               4127794
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.680
_shelx_estimated_absorpt_t_max   0.799
_shelx_res_checksum              98808
_shelx_hkl_checksum              37216