Icosahedral metallacarborane/carborane species derived from 1,1'-bis(o-carborane).
Thiripuranathar, Gobika; Man, Wing Y.; Palmero, Cesar; Chan, Antony P. Y.; Leube, Bernhard T.; Ellis, David; McKay, David; Macgregor, Stuart A.; Jourdan, Laure; Rosair, Georgina M.; Welch, Alan J.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 5628–5637; doi:10.1039/c5dt00081e

data_7033938
_publ_section_title
;
 Icosahedral metallacarborane/carborane species derived from
 1,1'-bis(o-carborane).
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5628
_journal_page_last               5637
_journal_paper_doi               10.1039/c5dt00081e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C4 H21 B19, C10 H16 N'
_chemical_formula_sum            'C14 H38 B19 N'
_chemical_formula_weight         425.84
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2015-01-08 deposited with the CCDC.
2015-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.068(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.851(9)
_cell_length_b                   10.072(4)
_cell_length_c                   13.477(6)
_cell_measurement_reflns_used    453
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.296
_cell_measurement_theta_min      2.829
_cell_volume                     2539.4(19)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.594
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2172
_diffrn_reflns_av_unetI/netI     0.1915
_diffrn_reflns_Laue_measured_fraction_full 0.594
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14879
_diffrn_reflns_point_group_measured_fraction_full 0.594
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         20.838
_diffrn_reflns_theta_min         1.088
_exptl_absorpt_coefficient_mu    0.052
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.4484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1145 before and 0.0877 after correction.
The Ratio of minimum to maximum transmission is 0.6022.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         2651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.2026
_refine_ls_R_factor_gt           0.0867
_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^)+(0.1143P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.2451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1229
_reflns_number_total             2651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00081e2.cif
_cod_data_source_block           x82895m
_cod_depositor_comments
'Adding full bibliography for 7033938--7033942.cif.'
_cod_original_cell_volume        2540(2)
_cod_database_code               7033938
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(B12)=Sof(H12)=1-FVAR(1)
 Sof(B3)=Sof(H3)=FVAR(1)
 Fixed Uiso: B3(0.03) B12(0.03)
3.a Secondary CH2 refined with riding coordinates:
 C103(H10J,H10K)
3.b Aromatic/amide H refined with riding coordinates:
 C107(H107), C106(H106), C108(H108), C105(H105), C109(H109)
3.c Idealised Me refined as rotating group:
 C102(H10A,H10B,H10C), C101(H10D,H10E,H10F), C100(H10G,H10H,H10I)
3.d Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4), B5(H5), B6(H6), C8(H8), B9(H9), B10(H10),
 B11(H11), B12(H12), C2'(H2'), B3'(H3'), B4'(H4'), B5'(H5'), B6'(H6'), B7'(H7'),
  B8'(H8'), B9'(H9'), B10'(H10'), B11'(H11'), B12'(H12')
;
_shelx_res_checksum              89484