Pathway bifurcations in the cage rearrangement of metallacarboranes: experimental and computational evidence.
Vinogradov, Mikhail M.; Nesterov, Ivan D.; Nelyubina, Yulia V.; Pavlov, Alexander A.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 287–293; doi:10.1039/d0dt03538f

data_7706019
_publ_section_title
;
 Pathway bifurcations in the cage rearrangement of metallacarboranes:
 experimental and computational evidence.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              287
_journal_page_last               293
_journal_paper_doi               10.1039/d0dt03538f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C15 H32 B9 Ir S'
_chemical_formula_sum            'C15 H32 B9 Ir S'
_chemical_formula_weight         533.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-09-22 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.389(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.9917(14)
_cell_length_b                   14.5337(12)
_cell_length_c                   16.3704(13)
_cell_measurement_reflns_used    9849
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.43
_cell_volume                     3988.5(6)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            63723
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.215
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.796
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2008/2 (Bruker,2010) was used for absorption correction.

Final HKLF 4 output contains 138199 reflections, Rint = 0.0490
 (44950 with I > 3sig(I), Rint = 0.0359)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       prism
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.186
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         7844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0166
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+5.1696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0374
_refine_ls_wR_factor_ref         0.0399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6862
_reflns_number_total             7844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03538f2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7706017--7706019.cif.'
_cod_database_code               7706019
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 B3(H3), B5(H5), B6(H6), B7(H7), B9(H9), B10(H10), B11(H11), B12(H12),
 B3A(H3A), B5A(H5A), B6A(H6A), B7A(H7A), B9A(H9A), B10A(H10A), B11A(H11A),
 B12A(H12A)
2.b Ternary CH refined with riding coordinates:
 C18(H18), C19(H19), C22(H22), C23(H23), C19A(H19A), C22A(H22A), C23A(H23A),
 C27A(H27A)
2.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C20(H20A,H20B), C21(H21A,
 H21B), C24(H24A,H24B), C25(H25A,H25B), C13A(H13C,H13D), C14A(H14C,H14D),
 C15A(H15C,H15D), C20A(H20C,H20D), C21A(H21C,H21D), C24A(H24C,H24D), C25A(H25C,
 H25D)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C16A(H16D,H16E,H16F), C17A(H17D,
 H17E,H17F)
;
_shelx_res_checksum              37322
_olex2_submission_special_instructions 'No special instructions were received'