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_1556683
_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_moiety         'C9 H25 B10 Cl2 N2 Sb'
_chemical_formula_sum            'C9 H25 B10 Cl2 N2 Sb'
_chemical_formula_weight         462.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 103.29(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.796(16)
_cell_length_b                   8.141(3)
_cell_length_c                   18.666(8)
_cell_measurement_reflns_used    10766
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      2.621
_cell_volume                     3963(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXL-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_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  0.0260
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10766
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.621
_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    1.656
_exptl_absorpt_correction_T_max  0.7730
_exptl_absorpt_correction_T_min  0.6972
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         4034
_refine_ls_number_restraints     541
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+8.0715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0602
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3813
_reflns_number_total             4034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2019-7-41.cif
_cod_data_source_block           fe0145_a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1556683
_shelx_res_checksum              50473
_shelx_hkl_checksum              78722