Efficient synthesis of carborane azo derivatives and their reactivity.
Gao, Yang; Lin, Yue-Jian; Han, Ying-Feng; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1585–1592; doi:10.1039/c6dt04550b

data_7041546
_publ_section_title
;
 Efficient synthesis of carborane azo derivatives and their reactivity.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1585
_journal_page_last               1592
_journal_paper_doi               10.1039/c6dt04550b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C25 H37 B10 Ir N2 O Se'
_chemical_formula_weight         760.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-24 deposited with the CCDC.
2016-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.743(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.445(3)
_cell_length_b                   23.872(7)
_cell_length_c                   12.067(4)
_cell_measurement_reflns_used    5598
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.54
_cell_measurement_theta_min      2.29
_cell_volume                     3103.1(16)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21213
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.795
_diffrn_reflns_theta_min         1.986
_exptl_absorpt_coefficient_mu    5.499
_exptl_absorpt_correction_T_max  0.491
_exptl_absorpt_correction_T_min  0.344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.855
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6569
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0869P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5023
_reflns_number_total             6569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04550b2.cif
_cod_data_source_block           6c
_cod_depositor_comments
'Adding full bibliography for 7041541--7041547.cif.'
_cod_original_cell_volume        3102.9(15)
_cod_database_code               7041546
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.391
_shelx_estimated_absorpt_t_max   0.609
_shelx_res_checksum              37532