Borole-based half-sandwich complexes of germanium and tin
Sarcevic, Julijan; Heitkemper, Tobias; Sindlinger, Christian P.; Chemical Communications  (2021) –; doi:10.1039/D1CC06227A

data_7129360
_publ_section_title
;
 Borole-based half-sandwich complexes of germanium and tin
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06227A
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_sum            'C73 H104 B2 Cl2 Ge2 N4 Si4'
_chemical_formula_weight         1387.66
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
FinalCif V89 by Daniel Kratzert, Freiburg 2021,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2021-11-02 deposited with the CCDC.	2021-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.172(3)
_cell_length_b                   18.172(3)
_cell_length_c                   11.769(3)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.9315
_cell_measurement_theta_min      2.2415
_cell_volume                     3886.4(13)
_computing_cell_refinement       'SAINT V8.40A'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'SAINT V8.40A'
_computing_molecular_graphics
'ORTEP (Farrugia, 2012), ShelXle (Hu\"bschle, 2011)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            103383
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         1.585
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.97
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction:
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48
(2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.418
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 1884 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4667
_refine_ls_number_restraints     631
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0241P)^2^+1.4723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0622
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4446
_reflns_number_total             4667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06227a2.cif
_cod_data_source_block           sad_a
_cod_original_cell_volume        3886.4(17)
_cod_database_code               7129360
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.694
_shelx_estimated_absorpt_t_max   0.928
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream'
_shelx_res_checksum              36115