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_4127796
_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            'C65 H78 Ge2 P2'
_chemical_formula_weight         1066.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 91.120(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8251(4)
_cell_length_b                   28.5433(10)
_cell_length_c                   18.1586(6)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.52
_cell_measurement_theta_min      2.29
_cell_volume                     5609.6(3)
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            64643
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.614
_diffrn_reflns_theta_min         1.815
_exptl_absorpt_coefficient_mu    1.168
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       prism
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.487
_refine_diff_density_min         -1.443
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 6805 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1249
_refine_ls_number_reflns         22560
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+14.6002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    0.951
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                17793
_reflns_number_total             22560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13645_si_003.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;

2020-08-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C130 H156 Ge4 P4'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2132.78
_cod_database_code               4127796
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0
_shelx_estimated_absorpt_t_max   0
_shelx_res_checksum              12237
_shelx_hkl_checksum              28318