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_7701725
_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         'C61 H63 Cl3 Co Ir N5 O9 P3 Ru, C H2 Cl2'
_chemical_formula_sum            'C62 H65 Cl5 Co Ir N5 O9 P3 Ru'
_chemical_formula_weight         1646.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-29
_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                90
_cell_angle_beta                 101.0227(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4813(2)
_cell_length_b                   29.6101(6)
_cell_length_c                   16.4218(2)
_cell_measurement_reflns_used    14782
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      75.3190
_cell_measurement_theta_min      4.9410
_cell_volume                     6434.36(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega   80.00  178.00   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   30.0000   90.0000 140

  2 omega  -49.00   35.00   0.7000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953   37.0000   60.0000 120

  3 omega   24.00   97.50   0.7000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6953 -125.0000  -30.0000 105

  4 omega   12.00  114.90   0.7000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6953   57.0000 -150.0000 147

  5 omega   26.00  108.60   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -94.0000  -30.0000 118

  6 omega   33.00   91.80   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  -90.0000 84

  7 omega   36.00   98.30   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -45.0000  -30.0000 89

  8 omega   94.00  178.00   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  125.0000   30.0000 120

  9 omega   15.00  117.20   0.7000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6953   37.0000  120.0000 146

 10 omega    7.00  119.00   0.7000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6953   77.0000  -30.0000 160

 11 omega   77.00  104.30   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000  -90.0000 39
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28631
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.999
_diffrn_reflns_theta_min         4.482
_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    10.901
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         11285
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+5.4858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9766
_reflns_number_total             11285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00244h2.cif
_cod_data_source_block           benson23a
_cod_original_cell_volume        6434.3(2)
_cod_database_code               7701725
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C20A-C19A = C20-C19
 1.52 with sigma of 0.02
 Cl2S-C1SA = Cl2S-C1S = Cl1A-C1SA = Cl1S-C1S
 1.72 with sigma of 0.02
 C22A-C21A = C22-C21
 1.52 with sigma of 0.02
 O6A-C21A
 1.4 with sigma of 0.02
 O3A-C15A
 1.4 with sigma of 0.02
 C16A-C15A
 1.5 with sigma of 0.02
 P0AA-C21A
 2.6 with sigma of 0.04
 O1-C11 \\sim O1A-C11
 with sigma of 0.02
 O2-C13 \\sim O2A-C13
 with sigma of 0.02
 O5-C19 \\sim O5A-C19A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1SA) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.002
Uanis(C1S) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(O6A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(P8) \\sim Ueq, Uanis(P0AA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
Uanis(O5A) \\sim Ueq, Uanis(O4A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.003
Uanis(O2A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.003
Uanis(O3A) \\sim Ueq, Uanis(C15A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.003
Uanis(C16A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.003
4. Rigid body (RIGU) restrains
 Cl1A, C1SA
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.002
 O6, C21, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O6A, C21A, C22A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O5A, C19A, C20A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O5, C19, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3, C15, C16
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 O3A, C15A, C16A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 P1, O1A, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: P0AA(0.1) P2(0.9) P3(0.9) P8(0.1) O1(0.9) O1A(0.1) O2(0.9)
 O2A(0.1) O3(0.9) O3A(0.1) O4(0.9) O4A(0.1) O5(0.9) O5A(0.1) O6(0.9) O6A(0.1)
 H11A(0.9) H11B(0.9) H11C(0.1) H11D(0.1) H13A(0.9) H13B(0.9) H13C(0.1)
 H13D(0.1) C15(0.9) H15A(0.9) H15B(0.9) C15A(0.1) H15C(0.1) H15D(0.1) C16(0.9)
 H16A(0.9) H16B(0.9) H16C(0.9) C16A(0.1) H16D(0.1) H16E(0.1) H16F(0.1)
 H17A(0.9) H17B(0.9) H17C(0.1) H17D(0.1) C19(0.75) H19A(0.75) H19B(0.75)
 C19A(0.25) H19C(0.25) H19D(0.25) C20(0.75) H20A(0.75) H20B(0.75) H20C(0.75)
 C20A(0.25) H20D(0.25) H20E(0.25) H20F(0.25) C21(0.66667) H21A(0.66667)
 H21B(0.66667) C21A(0.33333) H21C(0.33333) H21D(0.33333) C22(0.66667)
 H22A(0.66667) H22B(0.66667) H22C(0.66667) C22A(0.33333) H22D(0.33333)
 H22E(0.33333) H22F(0.33333) Cl1A(0.15) Cl1S(0.85) C1S(0.7) H1SA(0.7) H1SB(0.7)
 C1SA(0.3) H1SC(0.3) H1SD(0.3)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C11(H11C,H11D), C13(H13A,H13B), C13(H13C,H13D), C15(H15A,
 H15B), C15A(H15C,H15D), C17(H17A,H17B), C17(H17C,H17D), C19(H19A,H19B),
 C19A(H19C,H19D), C21(H21A,H21B), C21A(H21C,H21D), C1S(H1SA,H1SB), C1SA(H1SC,
 H1SD)
6.b 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.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C16A(H16D,H16E,
 H16F), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C20A(H20D,H20E,H20F),
 C22(H22A,H22B,H22C), C22A(H22D,H22E,H22F)
;
_shelx_res_checksum              502
_olex2_submission_special_instructions 'No special instructions were received'