PM-IRRAS and DFT investigation of the surface orientation of new Ir piano-stool complexes attached to Au (111)
Kubiak, Clifford P.; Miller, Christopher J.; Brunner, Felix M.; Kelly, H. Ray; Cheung, Po Ling; Torquato, Nicole A.; Gembicky, Milan; Okuno, Saya; Chan, Thomas; Batista, Victor S.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02730E

data_7711661
_publ_section_title
;
 PM-IRRAS and DFT investigation of the surface orientation of new Ir
 piano-stool complexes attached to Au (111)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02730E
_journal_year                    2022
_chemical_formula_moiety
'C63 H66 Ir3 N3 S3, 2.942(C6 H4 Cl2), C5.016 H3.344 Cl1.58'
_chemical_formula_sum            'C85.66 H81.11 Cl7.46 Ir3 N3 S3'
_chemical_formula_weight         2089.84
_chemical_name_systematic        Ir3N3S3C66
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-03
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.03.08 svn.r54f81f84 for OlexSys, GUI svn.r6485)
;
_audit_update_record
;
2022-07-25 deposited with the CCDC.	2022-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.978(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   45.563(8)
_cell_length_b                   18.693(3)
_cell_length_c                   21.023(4)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.549
_cell_measurement_theta_min      2.263
_cell_volume                     17903(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1623
_diffrn_reflns_av_unetI/netI     0.1008
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            104645
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.414
_diffrn_reflns_theta_max         24.414
_diffrn_reflns_theta_min         1.520
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.784
_exptl_absorpt_correction_T_max  0.2586
_exptl_absorpt_correction_T_min  0.1282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1289 before and 0.1000 after correction.
The Ratio of minimum to maximum transmission is 0.4957.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       needle
_exptl_crystal_F_000             8175
_exptl_crystal_preparation
'Stirred IrCp*Cl3 with potassium acetate and the disulfide ligand'
_exptl_crystal_recrystallization_method
'vapor diffusion of pentane into Ortho-dichlorobenzene'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.327
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         14729
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0410P)^2^+11.5852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9763
_reflns_number_total             14729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02730e2.cif
_cod_data_source_block           felix_ir2_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        17902(5)
_cod_database_code               7711661
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.646
_shelx_estimated_absorpt_t_min   0.328
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 Cl7S, Cl8S, C19S, C20S, C21S, C22S, C23S, C24S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 C14S, C13S, C18S, C17S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N3, C5B, C4B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Others
 Sof(Cl8S)=Sof(C19S)=Sof(C20S)=Sof(H20S)=Sof(C21S)=Sof(H21S)=Sof(C22S)=
 Sof(H22S)=Sof(C23S)=Sof(H23S)=Sof(C24S)=FVAR(1)
 Sof(Cl5S)=Sof(Cl6S)=Sof(C13S)=Sof(C14S)=Sof(H14S)=Sof(C15S)=Sof(H15S)=
 Sof(C16S)=Sof(H16S)=Sof(C17S)=Sof(H17S)=Sof(C18S)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C1A(H1A), C1B(H1B), C2(H2), C2A(H2A), C2B(H2B), C4(H4), C4A(H4A),
 C4B(H4B), C7(H7), C7A(H7A), C7B(H7B), C8(H8), C8A(H8A), C8B(H8B), C9(H9),
 C9A(H9A), C9B(H9B), C10(H10), C10A(H10A), C10B(H10B), C8S(H8S), C9S(H9S),
 C10S(H10S), C11S(H11S), C20S(H20S), C21S(H21S), C22S(H22S), C23S(H23S),
 C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C14S(H14S), C15S(H15S), C16S(H16S),
 C17S(H17S)
4.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C13A(H13D,H13E,H13F), C13B(H13G,H13H,H13I), C15(H15A,
 H15B,H15C), C15A(H15D,H15E,H15F), C15B(H15G,H15H,H15I), C17(H17A,H17B,H17C),
 C17A(H17D,H17E,H17F), C17B(H17G,H17H,H17I), C19(H19A,H19B,H19C), C19A(H19D,
 H19E,H19F), C19B(H19G,H19H,H19I), C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F),
 C21B(H21G,H21H,H21I)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              55906
_shelx_hkl_checksum              15424
_shelx_fab_checksum              51287
_olex2_exptl_crystal_mounting_method 'paratone on loop'
_olex2_submission_special_instructions 'No special instructions were received'