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_4341603
_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_absolute_configuration unk
_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      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 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                90.00
_cell_angle_beta                 91.5207(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.89037(14)
_cell_length_b                   10.47959(19)
_cell_length_c                   17.1104(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1414.32(4)
_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 10.4391
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22035
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.78
_diffrn_reflns_theta_min         1.94
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.902
_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    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         9033
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.2100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                8211
_reflns_number_total             9033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502265g_si_002.cif
_cod_data_source_block           4b
_cod_database_code               4341603
_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:
 C6(H6), C11(H11A), C4(H4), C10(H10A), C12(H12), C13(H13), C3(H3), C5(H5)
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:
 C14(H14), C7(H7), B4(H4A), B13(H13A), B21(H21), B20(H20), B10(H10), B5(H5A),
 B6(H6A), B11(H11), B16(H16), B17(H17), B18(H18), B3(H3A), B9(H9), B8(H8),
 B15(H15), B7(H7A), B2(H2), B14(H14A), B22(H22), B19(H19)
;