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_7706018
_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 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 94.072(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7089(9)
_cell_length_b                   15.4832(18)
_cell_length_c                   17.075(2)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      2.39
_cell_volume                     2032.9(4)
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19576
_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         1.777
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.667
_exptl_absorpt_correction_T_max  0.4806
_exptl_absorpt_correction_T_min  0.1218
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0505 before and 0.0451 after correction.
The Ratio of minimum to maximum transmission is 0.2534.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_description       prism
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.951
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0185
_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^)+(0.0174P)^2^+2.4299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0415
_refine_ls_wR_factor_ref         0.0426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3630
_reflns_number_total             4002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03538f2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7706017--7706019.cif.'
_cod_database_code               7706018
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.335
_shelx_estimated_absorpt_t_min   0.196
_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), B8(H8), B10(H10), B11(H11), B12(H12)
2.b Ternary CH refined with riding coordinates:
 C18(H18), C19(H19), C22(H22), C23(H23)
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)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              78636
_olex2_submission_special_instructions 'No special instructions were received'