Rapid Synthesis of Redox-Active Dodecaborane B12(OR)12 Clusters Under Ambient Conditions
Alex I. Wixtrom; Yanwu Shao; Dahee Jung; Charles W. Machan; Shaunt N. Kevork; Elaine A. Qian; Jonathan C. Axtell; Saeed I. Khan; Clifford P. Kubiak; Alexander M. Spokoyny; Inorganic Chemistry Frontiers 3 (2016) 711–717; doi:10.1039/C5QI00263J

data_4345982
_publ_section_title
;
 Rapid Synthesis of Redox-Active Dodecaborane B12(OR)12 Clusters Under
 Ambient Conditions
;
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              711
_journal_page_last               717
_journal_paper_doi               10.1039/C5QI00263J
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C108 H60 B12 F72 O12, C16 H36 N'
_chemical_formula_sum            'C124 H96 B12 F72 N O12'
_chemical_formula_weight         3289.73
_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
_cell_angle_alpha                90
_cell_angle_beta                 97.1607(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9085(3)
_cell_length_b                   38.6574(7)
_cell_length_c                   25.4370(4)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.36
_cell_measurement_theta_min      2.88
_cell_volume                     13569.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.1302
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            124864
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.508
_diffrn_reflns_theta_min         2.090
_diffrn_source                   'I\mS micro--focus source'
_exptl_absorpt_coefficient_mu    1.515
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       prism
_exptl_crystal_F_000             6604
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.06(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4384
_refine_ls_number_reflns         48036
_refine_ls_number_restraints     16471
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0890
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1641P)^2^+3.4272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2408
_refine_ls_wR_factor_ref         0.2551
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                40722
_reflns_number_total             48036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            NIHMS765968-supplement-Crystal_Data-2.cif
_cod_data_source_block           2
_cod_database_code               4345982
_shelx_estimated_absorpt_t_min   0.752
_shelx_estimated_absorpt_t_max   0.805
_shelxl_version_number           2014-3
_shelx_res_checksum              2626