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

data_7129355
_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_formula_sum            'C60 H92 B2 Cl2 Li4 O2 Si4'
_chemical_formula_weight         1077.97
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
FinalCif V86 by Daniel Kratzert, Freiburg 2021,
https://github.com/dkratzert/FinalCif
;
_audit_update_record
;
2021-11-02 deposited with the CCDC.	2021-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.751(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.109(2)
_cell_length_b                   14.636(2)
_cell_length_c                   15.670(2)
_cell_measurement_reflns_used    5987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.039
_cell_measurement_theta_min      2.3795
_cell_volume                     3235.6(8)
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_number            6409
_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         26.076
_diffrn_reflns_theta_min         1.904
_diffrn_source_current           0.98
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.745317
_exptl_absorpt_correction_T_min  0.632831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1: 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    1.106
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.467
_exptl_crystal_size_mid          0.413
_exptl_crystal_size_min          0.329
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0445P)^2^+2.5300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1045
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5227
_reflns_number_total             6409
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
'The data was integrated as a 2-component twin.'
_twin_individual_id              2
_twin_individual_twin_matrix_11  0.00052
_twin_individual_twin_matrix_12  0.89382
_twin_individual_twin_matrix_13  -0.10818
_twin_individual_twin_matrix_21  -1.0
_twin_individual_twin_matrix_22  0.00062
_twin_individual_twin_matrix_23  0.00102
_twin_individual_twin_matrix_31  0.00111
_twin_individual_twin_matrix_32  0.10818
_twin_individual_twin_matrix_33  1.1057
_cod_data_source_file            d1cc06227a2.cif
_cod_data_source_block           JS102
_cod_original_cell_volume        3235.5(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7129355
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.907
_shelx_estimated_absorpt_t_max   0.934
_shelx_res_checksum              89693