Synthesis and Structural Characterization of Two New Main Group Element Carboranylamidinates
Liebing, P.; Harmgarth, N.; Zorner, F.; Engelhardt, F.; Hilfert, L.; Busse, S.; Edelmann, F.T.; Inorganics 7 (2019) 41–; doi:10.3390/inorganics7030041

data_1556682
_publ_section_title
;
 Synthesis and Structural Characterization of Two New Main Group Element
 Carboranylamidinates
;
_journal_name_full               Inorganics
_journal_page_first              41
_journal_paper_doi               10.3390/inorganics7030041
_journal_volume                  7
_journal_year                    2019
_chemical_formula_sum            'C15 H33 B10 Cl Ge N2'
_chemical_formula_weight         457.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.166(4)
_cell_length_b                   11.279(5)
_cell_length_c                   12.294(3)
_cell_measurement_reflns_used    12110
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.185
_cell_measurement_theta_min      2.202
_cell_volume                     2241.6(13)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      ' 149 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12110
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.185
_diffrn_reflns_theta_min         2.202
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.491
_exptl_absorpt_correction_T_max  0.8903
_exptl_absorpt_correction_T_min  0.7397
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 2365 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.036(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5800
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+4.5754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.931
_reflns_number_gt                5643
_reflns_number_total             5800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2019-7-41.cif
_cod_data_source_block           fe0183_b
_cod_original_cell_volume        2241.8(12)
_cod_database_code               1556682
_shelx_res_checksum              17673
_shelx_hkl_checksum              52065