Carbolong chemistry: nucleophilic aromatic substitution of a triflate functionalized iridapentalene.
Li, Jinhua; Lu, Zhengyu; Hua, Yuhui; Chen, Dafa; Xia, Haiping; Chemical communications (Cambridge, England) 57 (2021) 8464–8467; doi:10.1039/d1cc03261e

data_7128731
_publ_section_title
;
 Carbolong chemistry: nucleophilic aromatic substitution of a triflate
 functionalized iridapentalene.
;
_journal_issue                   68
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8464
_journal_page_last               8467
_journal_paper_doi               10.1039/d1cc03261e
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C59 H49 Ir N O5 P2, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C61 H51 Cl2 F3 Ir N O9 P2 S'
_chemical_formula_weight         1356.12
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-17 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                87.5740(10)
_cell_angle_beta                 78.5770(10)
_cell_angle_gamma                86.1780(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3075(4)
_cell_length_b                   14.2370(5)
_cell_length_c                   14.8738(5)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.28
_cell_volume                     2754.79(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            70599
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.573
_diffrn_reflns_theta_min         2.284
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.687
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.643
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.976
_refine_diff_density_min         -2.635
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         12678
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+20.5596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10877
_reflns_number_total             12678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03261e2.cif
_cod_data_source_block           ljh200808_12_0m
_cod_depositor_comments
'Adding full bibliography for 7128726--7128732.cif.'
_cod_database_code               7128731
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.643
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl3) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(Cl0A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C0AA(H0AA,H0AB)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C00F(H00F), C7(H7), C3(H3), C00R(H00R), C00T(H00T), C00U(H00U),
 C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C010(H010), C011(H011),
 C013(H013), C014(H014), C015(H015), C017(H017), C019(H019), N1(H1A),
 C01B(H01B), C01C(H01C), C01D(H01D), C01F(H01F), C01G(H01G), C01H(H01H),
 C01I(H01I), C01J(H01J), C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O),
 C17(H17), C01S(H01S), C22(H22), C01V(H01V), C01Z(H01Z), C21(H21), C19(H19),
 C20(H20)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              47729
_shelx_hkl_checksum              41464
_shelx_fab_checksum              46301
_olex2_submission_special_instructions 'No special instructions were received'