A D3h-symmetry hexaazatriphenylene-tris-N-heterocyclic carbene ligand and its coordination to iridium and gold: preliminary catalytic studies.
Ibáñez, S; Poyatos, M.; Peris, E.; Chemical communications (Cambridge, England) 53 (2017) 3733–3736; doi:10.1039/c7cc00525c

data_7119708
_publ_section_title
;
 A D3h-symmetry hexaazatriphenylene-tris-N-heterocyclic carbene ligand and
 its coordination to iridium and gold: preliminary catalytic studies.
;
_journal_issue                   26
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3733
_journal_page_last               3736
_journal_paper_doi               10.1039/c7cc00525c
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety
'3(C10 H8 Cl2.4 I0.6 Ru), 3(C0.87 H1.74 Cl1.78), C49 H48 N12, 0.98(C3 O3)'
_chemical_formula_sum            'C84.56 H83.22 Cl12.57 I1.8 N12 O2.95 Ru3'
_chemical_formula_weight         2292.12
_chemical_name_systematic        str1788
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-01-19 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.7983(7)
_cell_length_b                   17.7983(7)
_cell_length_c                   32.0239(18)
_cell_measurement_reflns_used    4312
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.9520
_cell_measurement_theta_min      3.4060
_cell_volume                     8785.4(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -79.00  102.30   0.7000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9725    0.0000 -180.0000 259

  2 omega  -65.00   -9.70   0.7000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9725  -57.0000 -180.0000 79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            15067
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         3.445
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       prism
_exptl_crystal_F_000             3418
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, methanol, hexane'
_exptl_crystal_size_max          0.2212
_exptl_crystal_size_mid          0.1837
_exptl_crystal_size_min          0.0356
_refine_diff_density_max         1.907
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details
;
 Flack x determined using 1866 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.043(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6958
_refine_ls_number_restraints     405
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0830
_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^)+(0.1690P)^2^+14.5310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2163
_refine_ls_wR_factor_ref         0.2427
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                5570
_reflns_number_total             6958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00525c2.cif
_cod_data_source_block           str1788_sq
_cod_depositor_comments          'Adding full bibliography for 7119708.cif.'
_cod_original_cell_volume        8785.4(8)
_cod_original_formula_sum        'C84.56 H83.22 Cl12.57 I1.80 N12 O2.95 Ru3'
_cod_database_code               7119708
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.736(4) 0.264(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C2-C3 = C4-C5
 1.54 with sigma of 0.02
 C3-C4
 1.54 with sigma of 0.002
 C20-C19 \\sim C19-C18
 with sigma of 0.02
 C2-C3 \\sim C4-C5
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: I1(0.6) C28(0.87) H28A(0.87) H28B(0.87) Cl1(0.4) O2(0.65)
 C30(0.33333) C29(0.65)
7.a Ternary CH refined with riding coordinates:
 C19(H19)
7.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C28(H28A,H28B), C8(H8A,H8B), C7(H7A,H7B), C2(H2A,H2B), C3(H3A,H3B)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C12(H12), C13(H13), C26(H26), C27(H27), C22(H22), C23(H23)
7.d Fitted hexagon refined as free rotating group:
 C26(C27,C21,C22,C23,C24)
7.e Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              56887
_shelx_hkl_checksum              55903
_shelx_fab_checksum              96443
_olex2_submission_special_instructions 'No special instructions were received'