Triazole vs. triazolium carbene ligands in the site-selective cyclometallation of o-carboranes by M(iii) (M = Ir, Rh) complexes.
Frutos, María; Gómez-Gallego, Mar; Giner, Elena A.; Sierra, Miguel A.; Ramírez de Arellano, Carmen; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9975–9979; doi:10.1039/c8dt02296h

data_7046898
_publ_section_title
;
 Triazole vs. triazolium carbene ligands in the site-selective
 cyclometallation of o-carboranes by M(iii) (M = Ir, Rh) complexes.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9975
_journal_page_last               9979
_journal_paper_doi               10.1039/c8dt02296h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C22 H35 B10 Cl Ir N3'
_chemical_formula_weight         677.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-05-04 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.5605(9)
_cell_length_b                   8.6073(2)
_cell_length_c                   20.2755(5)
_cell_measurement_reflns_used    9164
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.1500
_cell_measurement_theta_min      3.4920
_cell_volume                     5507.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalMaker 9.2.9 (1994-2017)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'SuperNova, Oxford Diffraction'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_unetI/netI     0.0909
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43285
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         31.975
_diffrn_reflns_theta_min         3.279
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.964
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro (Rigaku Oxford Diff., 2015)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         6.280
_refine_diff_density_min         -1.842
_refine_diff_density_rms         0.233
_refine_ls_abs_structure_details
; 
 Flack x determined using 4170 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.001(8)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         15524
_refine_ls_number_restraints     979
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0351P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.706
_reflns_Friedel_fraction_full    0.781
_reflns_Friedel_fraction_max     0.690
_reflns_number_gt                12487
_reflns_number_total             15524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02296h2.cif
_cod_data_source_block           fp62bb
_cod_depositor_comments
'Adding full bibliography for 7046897--7046898.cif.'
_cod_database_code               7046898
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.469
_shelx_estimated_absorpt_t_max   0.755
_shelx_res_checksum              38418