Convenient Route to Monocarba-closo-dodecaborate Anions
Tanaka, Naoki; Shoji, Yoshiaki; Fukushima, Takanori; Organometallics 35 (2016) 2022–; doi:10.1021/acs.organomet.6b00309

data_4088692
_publ_section_title
;
 Convenient Route to Monocarba-closo-dodecaborate Anions
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2022
_journal_paper_doi               10.1021/acs.organomet.6b00309
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C4 H24 B9 N'
_chemical_formula_weight         183.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 100.2780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.4166(5)
_cell_length_b                   10.3935(8)
_cell_length_c                   9.5956(7)
_cell_measurement_reflns_used    4531
_cell_measurement_temperature    90
_cell_measurement_theta_max      29.18
_cell_measurement_theta_min      2.91
_cell_volume                     629.67(8)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHELL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0115
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4578
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.157
_exptl_absorpt_coefficient_mu    0.044
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.968
_exptl_crystal_description       block
_exptl_crystal_F_000             200
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.138
_refine_diff_density_min         -0.116
_refine_diff_density_rms         0.027
_refine_ls_abs_structure_details
;
 Flack x determined using 998 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.5(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2208
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0587P)^2^+0.0565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    0.959
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                2175
_reflns_number_total             2208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00309_si_002.cif
_cod_data_source_block           arachno_Me3NH
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4088692
_shelx_estimated_absorpt_t_min   0.990
_shelx_estimated_absorpt_t_max   0.995
_shelxl_version_number           2014/6
_shelx_res_checksum              73857
_shelx_hkl_checksum              23438