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_7701723
_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         'C69 H76 Cl2 Co Ir N5 O9 P3 Ru'
_chemical_formula_sum            'C75 H90 Cl2 Co Ir N5 O9 P3 Ru'
_chemical_formula_weight         1721.52
_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     iterative
_audit_creation_date             2018-04-26
_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                85.316(2)
_cell_angle_beta                 80.0763(19)
_cell_angle_gamma                78.870(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0825(3)
_cell_length_b                   13.8500(5)
_cell_length_c                   20.4656(5)
_cell_measurement_reflns_used    13938
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      75.4840
_cell_measurement_theta_min      4.5200
_cell_volume                     3579.54(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector_area_resol_mean 10.3587
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega   86.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   61.0000    0.0000 92

  2 omega  -68.00   32.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453   57.0000  -30.0000 100

  3 omega  -69.00   37.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453   77.0000   60.0000 106

  4 omega  -69.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453   57.0000 -150.0000 100

  5 omega   33.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000 -120.0000 82

  6 omega   40.00  135.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -61.0000  -60.0000 95

  7 omega  102.00  176.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  111.0000  -60.0000 74

  8 omega   32.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000  -30.0000 83

  9 omega   97.00  172.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   45.0000   60.0000 75

 10 omega   84.00  175.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   30.0000  120.0000 91

 11 omega   64.00  141.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -77.0000   30.0000 77

 12 omega   36.00   73.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -45.0000 -150.0000 37
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0729772000
_diffrn_orient_matrix_UB_12      0.0616251000
_diffrn_orient_matrix_UB_13      -0.0450722000
_diffrn_orient_matrix_UB_21      0.0129334000
_diffrn_orient_matrix_UB_22      -0.0713709000
_diffrn_orient_matrix_UB_23      -0.0560102000
_diffrn_orient_matrix_UB_31      -0.0963823000
_diffrn_orient_matrix_UB_32      0.0631834000
_diffrn_orient_matrix_UB_33      -0.0261896000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20356
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.499
_diffrn_reflns_theta_min         4.318
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    8.818
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.177
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         12629
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0500P)^2^+1.9500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11814
_reflns_number_total             12629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00244h2.cif
_cod_data_source_block           wai150cult
_cod_original_cell_volume        3579.55(17)
_cod_database_code               7701723
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 98.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C98-C97
 1.52 with sigma of 0.02
 C97-C96
 1.52 with sigma of 0.02
 C94-C93 = C95-C94
 1.52 with sigma of 0.02
 C96A-C94A
 2.3 with sigma of 0.02
 C94-C96
 2.3 with sigma of 0.02
 C98A-C91 \\sim C92A-C91 \\sim C96A-C92A \\sim C97A-C96A \\sim C98A-C97A \\sim
C93A-C92A \\sim C94A-
 C93A \\sim C95A-C94A \\sim C96A-C95A
 with sigma of 0.02
 C98-C97 \\sim C97-C96 \\sim C98-C91 \\sim C92-C91 \\sim C96-C92 \\sim C96-C95
\\sim C95-C94 \\sim C94-C93
 \\sim C93-C92
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C91) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C93A) \\sim Ueq, Uanis(C94A) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C95A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C91, C92A, C93A, C94A, C95A, C96A, C97A, C98A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.002
 C91, C92, C93, C94, C95, C96, C97, C98
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: H91(0.5) H91A(0.5) C92(0.5) H92(0.5) C92A(0.5) H92A(0.5) C93(0.5)
 H93A(0.5) H93B(0.5) C93A(0.5) H93C(0.5) H93D(0.5) C94(0.5) H94A(0.5) H94B(0.5)
 C94A(0.5) H94C(0.5) H94D(0.5) C95(0.5) H95A(0.5) H95B(0.5) C95A(0.5) H95C(0.5)
 H95D(0.5) C96(0.5) H96(0.5) C96A(0.5) H96A(0.5) C97(0.5) H97A(0.5) H97B(0.5)
 C97A(0.5) H97C(0.5) H97D(0.5) C98(0.5) H98A(0.5) H98B(0.5) C98A(0.5) H98C(0.5)
 H98D(0.5)
6.a Ternary CH refined with riding coordinates:
 C91(H91), C91(H91A), C92(H92), C92A(H92A), C96(H96), C96A(H96A)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,
 H19B), C21(H21A,H21B), C93(H93A,H93B), C93A(H93C,H93D), C94(H94A,H94B),
 C94A(H94C,H94D), C95(H95A,H95B), C95A(H95C,H95D), C97(H97A,H97B), C97A(H97C,
 H97D), C98(H98A,H98B), C98A(H98C,H98D)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C32(H32), C33(H33), C37(H37),
 C38(H38), C42(H42), C43(H43), C47(H47), C48(H48), 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)
6.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              29004
_shelx_fab_checksum              14591
_olex2_submission_special_instructions 'No special instructions were received'