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

data_7129356
_publ_section_title
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 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 N4 Si4 Sn2'
_chemical_formula_weight         1479.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_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            8
_cell_length_a                   25.802(3)
_cell_length_b                   25.796(3)
_cell_length_c                   23.532(2)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.5065
_cell_measurement_theta_min      2.233
_cell_volume                     15663(3)
_computing_cell_refinement       'SAINT V8.40A'
_computing_data_collection       "'Bruker Apex II'"
_computing_data_reduction        'SAINT V8.40A'
_computing_molecular_graphics    'ORTEP (L. J. Farrugia, 2012)'
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            111471
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.758
_diffrn_reflns_theta_min         1.116
_diffrn_source_current           0.98
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6702
_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    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             6160
_exptl_crystal_recrystallization_method 'from saturated toluene solutions'
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 7706 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.022(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         16679
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0216
_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^)+(0.0239P)^2^+2.0473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0503
_reflns_Friedel_coverage         0.948
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                16260
_reflns_number_total             16679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06227a2.cif
_cod_data_source_block           sad_iba2_a
_cod_original_cell_volume        15662(3)
_cod_database_code               7129356
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.876
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              44598