Chlorination of 1-Carba-closo-dodecaborate and 1-Ammonio-closo-dodecaborate Anions.
Saleh, Mahmoud; Powell, Douglas R.; Wehmschulte, Rudolf J.; Inorganic chemistry 55 (2016) 10617–10627; doi:10.1021/acs.inorgchem.6b01867

data_4349029
_publ_section_title
;
 Chlorination of 1-Carba-closo-dodecaborate and
 1-Ammonio-closo-dodecaborate Anions.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10617
_journal_page_last               10627
_journal_paper_doi               10.1021/acs.inorgchem.6b01867
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C9 H25.85 B12 Cl6.15 N, C8 H20 N'
_chemical_formula_sum            'C17 H45.85 B12 Cl6.15 N2'
_chemical_formula_weight         626.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 114.6508(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2771(16)
_cell_length_b                   17.981(3)
_cell_length_c                   19.097(3)
_cell_measurement_reflns_used    5229
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.18
_cell_volume                     3207.4(9)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'XP (Bruker, 2002)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36013
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.631
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       plate
_exptl_crystal_F_000             1305
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.165
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6313
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0650P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5114
_reflns_number_total             6313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01867_si_002.cif
_cod_data_source_block           '[Et4N][6]'
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349029
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              99401
_shelx_hkl_checksum              20583