Iridium porphyrin complexes with μ-nitrido, hydroxo, hydrosulfido and alkynyl ligands.
So, Shiu-Chun; Cheung, Wai-Man; Chiu, Wai-Hang; de Vere-Tucker, Matthew; Sung, Herman H.-Y.; Williams, Ian D.; Leung, Wa-Hung; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8340–8349; doi:10.1039/c9dt00244h

data_7701724
_publ_section_title
;
 Iridium porphyrin complexes with \m-nitrido, hydroxo, hydrosulfido and
 alkynyl ligands.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8340
_journal_page_last               8349
_journal_paper_doi               10.1039/c9dt00244h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C62 H44 Ir N4 P S'
_chemical_formula_sum            'C62 H44 Ir N4 P S'
_chemical_formula_weight         1100.24
_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             2018-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-05-01 deposited with the CCDC.	2019-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                97.827(3)
_cell_angle_beta                 98.001(3)
_cell_angle_gamma                107.838(4)
_cell_formula_units_Z            2
_cell_length_a                   10.0055(4)
_cell_length_b                   14.3928(6)
_cell_length_c                   17.7170(7)
_cell_measurement_reflns_used    8508
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.2520
_cell_measurement_theta_min      4.5330
_cell_volume                     2361.41(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     30.00 113.00   1.00    3.00    --  107.97-111.00  60.00   83
  2  \w   -116.00 -14.00   1.00    1.00    --  -40.45 -37.00 -30.00  102
  3  \w   -114.00 -11.00   1.00    1.00    --  -40.45 -57.00  90.00  103
  4  \w    -92.00  -3.00   1.00    1.00    --  -40.45 125.00-150.00   89
  5  \w     62.00 113.00   1.00    3.00    --  107.97-111.00-150.00   51
  6  \w    100.00 178.00   1.00    3.00    --  107.97 111.00  90.00   78
  7  \w     42.00  78.00   1.00    3.00    --  107.97 -45.00 -60.00   36
  8  \w     34.00 133.00   1.00    3.00    --  107.97 -61.00  60.00   99
  9  \w     90.00 132.00   1.00    3.00    --  107.97 -45.00 -60.00   42
 10  \w     53.00 178.00   1.00    3.00    --  107.97  15.00 -90.00  125
 11  \w     79.00 177.00   1.00    3.00    --  107.97  61.00 150.00   98
 12  \w     40.00 133.00   1.00    3.00    --  107.97 -61.00-180.00   93
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1604757000
_diffrn_orient_matrix_UB_12      0.0187196000
_diffrn_orient_matrix_UB_13      0.0013989000
_diffrn_orient_matrix_UB_21      -0.0164461000
_diffrn_orient_matrix_UB_22      0.0271757000
_diffrn_orient_matrix_UB_23      -0.0811390000
_diffrn_orient_matrix_UB_31      0.0337475000
_diffrn_orient_matrix_UB_32      0.1096645000
_diffrn_orient_matrix_UB_33      0.0375852000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13649
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.498
_diffrn_reflns_theta_min         3.766
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.193
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         8385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0290P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7660
_reflns_number_total             8385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00244h2.cif
_cod_data_source_block           wai212cult
_cod_original_cell_volume        2361.41(17)
_cod_database_code               7701724
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 98.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.46
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All S(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C17(H17), C18(H18), C22(H22), C23(H23), C27(H27),
 C28(H28), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55),
 C56(H56), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C72(H72), C73(H73),
  C74(H74), C75(H75), C76(H76), C82(H82), C83(H83), C84(H84), C85(H85),
 C86(H86), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96)
2.b Tetrahedral OH refined with riding coordinates:
 S1(H1)
;
_shelx_res_checksum              32406
_olex2_date_sample_data_collection 2018-06-25
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.225
_oxdiff_exptl_absorpt_empirical_full_min 0.874