Cooperative N-H bond activation by amido-Ge(ii) cations.
Zhou, Xueer; Vasko, Petra; Hicks, Jamie; Fuentes, M Ángeles; Heilmann, Andreas; Kolychev, Eugene L.; Aldridge, Simon; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9495–9504; doi:10.1039/d0dt01960g

data_7704711
_publ_section_title
;
 Cooperative N-H bond activation by amido-Ge(ii) cations.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9495
_journal_page_last               9504
_journal_paper_doi               10.1039/d0dt01960g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C16 Al F36 O4, C31 H33 Ge N P'
_chemical_formula_sum            'C47 H33 Al F36 Ge N O4 P'
_chemical_formula_weight         1490.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-05-22 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                83.214(3)
_cell_angle_beta                 88.694(2)
_cell_angle_gamma                87.381(2)
_cell_formula_units_Z            4
_cell_length_a                   12.1911(3)
_cell_length_b                   15.3762(6)
_cell_length_c                   29.9659(10)
_cell_measurement_reflns_used    12973
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.0850
_cell_measurement_theta_min      5.7740
_cell_volume                     5571.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            24700
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.701
_diffrn_reflns_theta_min         3.630
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.718
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.843
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1838
_refine_ls_number_reflns         24700
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0647
_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^)+(0.1321P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.1824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19220
_reflns_number_total             24700
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9971\% 
 around [1.00 0.00 0.00] (reciprocal) or [1.00 -0.03 -0.01] (direct)
;
_cod_data_source_file            d0dt01960g2.cif
_cod_data_source_block           334xzjh19_twin_comp1_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 7704706--7704714.cif.'
_cod_database_code               7704711
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.550
_shelx_estimated_absorpt_t_max   0.812
_oxdiff_twin_items               2
_oxdiff_twin_integration_method  simultaneous
_shelx_res_checksum              59923
_shelx_hkl_checksum              6722