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_7706017
_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         'C14 H30 B9 Ir O S'
_chemical_formula_sum            'C14 H30 B9 Ir O S'
_chemical_formula_weight         535.93
_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
_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                 97.3260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6152(4)
_cell_length_b                   15.4766(8)
_cell_length_c                   16.6390(8)
_cell_measurement_reflns_used    5507
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.47
_cell_volume                     1945.02(17)
_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)'
_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  0.0532
_diffrn_reflns_av_unetI/netI     0.0482
_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            16954
_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         26.999
_diffrn_reflns_theta_min         1.804
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.972
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.1993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1447 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.4603.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       prism
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0095P)^2^+0.1474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3442
_reflns_number_total             4247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03538f2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7706017--7706019.cif.'
_cod_database_code               7706017
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.275
_shelx_estimated_absorpt_t_min   0.229
_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:
 C17(H17), C18(H18), C21(H21), C22(H22)
2.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C19(H19A,H19B), C20(H20A,H20B), C23(H23A,
 H23B), C24(H24A,H24B)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              16155
_olex2_submission_special_instructions 'No special instructions were received'