Phospha-bicyclohexene-germylenes exhibiting unexpected reactivity.
Würdemann, Marie Sophie; Kühn, Steffen; Bötel, Tobias; Schmidtmann, Marc; Müller, Thomas; Chemical science 15 (2024) 14161–14170; doi:10.1039/d4sc04034a

data_1572213
_publ_section_title
;
 Phospha-bicyclohexene-germylenes exhibiting unexpected reactivity.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              14161
_journal_page_last               14170
_journal_paper_doi               10.1039/d4sc04034a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_structural     GeC4(CH3)2(Si(CH3)2(C4H9))2(C7H12N2)
_chemical_formula_sum            'C25 H48 Ge N2 Si2'
_chemical_formula_weight         505.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-06-17 deposited with the CCDC.	2024-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.0413(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0704(3)
_cell_length_b                   12.4659(3)
_cell_length_c                   21.0500(6)
_cell_measurement_reflns_used    9784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.23
_cell_measurement_theta_min      2.28
_cell_volume                     2851.18(13)
_computing_cell_refinement       'Bruker SAINT V8.40B'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Photon III CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            218320
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         40.248
_diffrn_reflns_theta_min         1.908
_diffrn_source                   'I\mS microfocus'
_exptl_absorpt_coefficient_mu    1.172
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         17959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0209
_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^)+(0.0250P)^2^+0.5500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15933
_reflns_number_total             17959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04034a3.cif
_cod_data_source_block           40b
_cod_depositor_comments
'Adding full bibliography for 1572207--1572213.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1572213
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.826
_shelx_estimated_absorpt_t_max   0.872
_shelx_res_checksum              8779
_shelx_hkl_checksum              19662