Synthesis and Characterization of 12-Pyridinium Derivatives of the [closo-1-CB11H12](-) Anion.
Pecyna, Jacek; Ringstrand, Bryan; Domagała, Sławomir; Kaszyński, Piotr; Woźniak, Krzysztof; Inorganic chemistry  (2014) 141113084747009–; doi:10.1021/ic502265g

data_4341602
_publ_section_title
;
 Synthesis and Characterization of 12-Pyridinium Derivatives of the
 [closo-1-CB11H12](-) Anion.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141113084747009
_journal_paper_doi               10.1021/ic502265g
_journal_year                    2014
_chemical_formula_moiety         'C7 H18 B11 N O'
_chemical_formula_sum            'C7 H18 B11 N O'
_chemical_formula_weight         251.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                87.461(2)
_cell_angle_beta                 77.206(2)
_cell_angle_gamma                77.472(2)
_cell_formula_units_Z            4
_cell_length_a                   10.1946(3)
_cell_length_b                   11.9855(3)
_cell_length_c                   12.0919(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1406.48(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XLMP (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 16.0026
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            44837
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.32
_diffrn_reflns_theta_min         1.73
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         9535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+0.5849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                7945
_reflns_number_total             9535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502265g_si_003.cif
_cod_data_source_block           1e
_cod_original_cell_volume        1406.47(6)
_cod_database_code               4341602
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C12(H12), C11(H11), C10(H10), C5(H5), C13(H13), C6(H6)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
2.c Boron cage BH refined with riding coordinates:
 B5(H5A), B7(H7), B1(H1), B12(H12A), B2(H2), B8(H8), B13(H13A), B21(H21),
 B3(H3A), B18(H18), B14(H14), B4(H4A), B16(H16), B22(H22), B15(H15), B20(H20),
 B10(H10A), B19(H19), B17(H17), B6(H6A), B11(H11A), B9(H9)
;