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_7704712
_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         'C30 H35 Ge N4, C16 Al F36 O4, 0.5(C6 H5 F)'
_chemical_formula_sum            'C49 H37.5 Al F36.5 Ge N4 O4'
_chemical_formula_weight         1539.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-09-07 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   80.2560(12)
_cell_length_b                   29.4338(5)
_cell_length_c                   10.7141(2)
_cell_measurement_reflns_used    56577
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.0610
_cell_measurement_theta_min      4.3900
_cell_volume                     25309.3(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (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 0.990
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       98
_diffrn_reflns_limit_h_min       -100
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            131887
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.137
_diffrn_reflns_theta_min         3.725
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.208
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       block
_exptl_crystal_F_000             12240
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.405
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.166
_refine_ls_abs_structure_details
;
 Flack x determined using 5621 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.650
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1116
_refine_ls_number_reflns         13230
_refine_ls_number_restraints     675
_refine_ls_restrained_S_all      1.792
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.1155
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3260
_refine_ls_wR_factor_ref         0.3316
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                12751
_reflns_number_total             13230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01960g2.cif
_cod_data_source_block           207xzjh18-F_a
_cod_depositor_comments
'Adding full bibliography for 7704706--7704714.cif.'
_cod_original_formula_sum        'C49 H37.50 Al F36.50 Ge N4 O4'
_cod_database_code               7704712
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.512
_shelx_estimated_absorpt_t_max   0.879
_shelx_res_checksum              37957
_shelx_hkl_checksum              21768