Formation and reactivity of a unique M⋯C-H interaction stabilized by carborane cages.
Liu, Xin-Ran; Cui, Peng-Fei; García-Rodeja, Yago; Solà, Miquel; Jin, Guo-Xin; Chemical science 15 (2024) 9274–9280; doi:10.1039/d4sc01158a

data_1571663
_publ_section_title
;
 Formation and reactivity of a unique M&#x22ef;C-H interaction stabilized
 by carborane cages.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              9274
_journal_page_last               9280
_journal_paper_doi               10.1039/d4sc01158a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C45 H79 B30 Ir3 N3 S3'
_chemical_formula_sum            'C45 H79 B30 Ir3 N3 S3'
_chemical_formula_weight         1658.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-10-03
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-10-25 deposited with the CCDC.	2024-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                91.778(2)
_cell_angle_beta                 91.812(2)
_cell_angle_gamma                103.9010(10)
_cell_formula_units_Z            4
_cell_length_a                   17.6388(6)
_cell_length_b                   18.5304(7)
_cell_length_c                   24.0367(9)
_cell_measurement_reflns_used    9088
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      52.16
_cell_measurement_theta_min      3.20
_cell_volume                     7616.5(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            125456
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        52.299
_diffrn_reflns_theta_max         52.299
_diffrn_reflns_theta_min         3.736
_diffrn_source_current           2.86
_diffrn_source_power             0.1999426
_diffrn_source_voltage           69.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.552
_exptl_absorpt_correction_T_max  0.008
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       block
_exptl_crystal_F_000             3196
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.618
_refine_diff_density_min         -1.691
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1549
_refine_ls_number_reflns         26018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0380P)^2^+42.7584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22443
_reflns_number_total             26018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01158a2.cif
_cod_data_source_block           230218d_0m_a
_cod_depositor_comments
;
Adding full bibliography for 1571656--1571663.cif.

2025-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C90 H158 B60 Ir6 N6 S6'
_cod_original_formula_weight         3318.37
_cod_original_formula_moiety         '2(C45 H79 B30 Ir3 N3 S3)'
_cod_original_formula_units_Z            2
_cod_database_code               1571663
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00Z(H00Z), C01M(H01M), C01Q(H01Q), C01S(H01S)
2.b Idealised Me refined as rotating group:
 C014(H01N,H01O,H01P), C017(H01A,H01B,H01C), C01V(H01D,H01E,H01F), C01W(H01G,
 H01H,H01I), C01X(H01J,H01K,H01L), C022(H1,H,HA), C023(H2,HB,HC), C027(H02A,
 H02B,H02C), C02B(H3,HD,HE), C02E(H4,HF,HG), C02G(H02G,H02H,H02I), C02H(H5,HH,
 HI), C02J(H02J,H02K,H02L), C02K(H7,HJ,HK), C02L(H8,HL,HM), C02M(H02M,H02N,
 H02O), C02T(H02T,H02U,H02V), C02U(H02W,H02X,H02Y), C02Y(H02,HN,HO), C031(H03A,
 H03B,H03C), C033(H03D,H03E,H03F), C03D(H03X,H03Y,HP), C03K(H03,HQ,HR),
 C03R(H03N,H03O,H03Q), C03W(H03R,H03S,H03V), C042(H04A,H04B,H04E), C048(H04F,
 H04H,H04I), C04H(H04O,H04P,H04Q), C04M(H04U,H04V,H04W), C04O(H04Y,HS,HT)
2.c Boron cage BH refined with riding coordinates:
 C00M(H00M), C00T(H00T), C01Y(H01Y), C029(H029), B02A(H02D), B02C(H02E),
 B02D(H02F), B02I(H6), B02N(H02P), B02O(H02Q), C02P(H02R), B02Q(H02S), B02S(H9),
  B02V(H10), B02W(H02Z), B02X(H11), C02Z(H12), B030(H030), B032(H032),
 B034(H034), B035(H035), B036(H036), B038(H038), B03A(H03G), B03B(H03W),
 B03C(H03H), B03E(H03I), B03F(H03J), B03G(H03Z), B03H(H03K), B03J(H03L),
 B03L(H03M), B03M(H13), B03N(H14), B03O(H15), B03P(H03P), B03S(H16), B03T(H03T),
  B03U(H03U), B03V(H17), B03X(H18), B03Z(H19), B040(H040), B041(H041),
 B043(H043), B044(H044), B045(H045), B046(H046), B047(H047), B049(H049),
 B04A(H04K), B04B(H04L), B04C(H04C), B04D(H04D), B04E(H04M), B04F(H04N),
 B04G(H04G), B04I(H04R), B04J(H04J), B04K(H04S), B04L(H04T), B04N(H04X)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90361
_shelx_fab_checksum              59705
_olex2_submission_special_instructions 'No special instructions were received'