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_7701728
_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_absolute_configuration ad
_chemical_formula_moiety         '2(C62 H45 Ir N4 O P), C4 H8 O, H2 O'
_chemical_formula_sum            'C128 H100 Ir2 N8 O4 P2'
_chemical_formula_weight         2260.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-04-15
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.2427(2)
_cell_length_b                   10.41332(13)
_cell_length_c                   35.1224(3)
_cell_measurement_reflns_used    19315
_cell_measurement_temperature    100.10(10)
_cell_measurement_theta_max      75.4910
_cell_measurement_theta_min      4.7390
_cell_volume                     9598.03(16)
_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      100.10(10)
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega   33.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000   60.0000 56

  2 omega   37.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000  120.0000 65

  3 omega   80.00  172.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   30.0000 -120.0000 92

  4 omega   57.00  139.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  178.0000  -90.0000 82

  5 omega   58.00  141.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  178.0000  120.0000 83

  6 omega   33.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000 -150.0000 38

  7 omega  -49.00   34.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0703   37.0000 -150.0000 83

  8 omega -114.00  -11.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0703  -57.0000   60.0000 103
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_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  0.0284
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            30575
_diffrn_reflns_point_group_measured_fraction_full 0.821
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.986
_diffrn_reflns_theta_min         4.206
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35
_diffrn_source_power             1.75
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.115
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62828
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             4560
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.398
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 4941 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1405
_refine_ls_number_reflns         14064
_refine_ls_number_restraints     247
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+5.2018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.633
_reflns_Friedel_fraction_full    0.647
_reflns_Friedel_fraction_max     0.648
_reflns_number_gt                13582
_reflns_number_total             14064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00244h2.cif
_cod_data_source_block           benson47cult
_cod_original_cell_volume        9598.03(17)
_cod_database_code               7701728
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1WA,H1WB} of O1W, {H1AA,H1AB} of O1A, All C(H,H) groups
 At 1.5 times of:
  {H1A,H1B} of O1
2. Restrained distances
 C82A-C81A \\sim C83A-C82A \\sim C83A-C84A \\sim C84A-C85A \\sim C85A-C86A
\\sim C81A-C86A
 with sigma of 0.02
 C82B-C81B \\sim C83B-C82B \\sim C83B-C84B \\sim C84B-C85B \\sim C85B-C86B
\\sim C81B-C86B
 with sigma of 0.02
 C21A-C26A \\sim C21A-C22A \\sim C22A-C23A \\sim C24A-C23A \\sim C25A-C24A
\\sim C25A-C26A
 with sigma of 0.02
 C21B-C22B \\sim C22B-C23B \\sim C24B-C23B \\sim C25B-C24B \\sim C25B-C26B
\\sim C21B-C26B
 with sigma of 0.02
3. Restrained planarity
 C81A, C82A, C83A, C84A, C85A, C86A
 with sigma of 0.1
 C81B, C82B, C83B, C84B, C85B, C86B
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 P1A, C81B, C82B, C83B, C84B, C85B, C86B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1A, C21B, C22B, C23B, C24B, C25B, C26B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P1A, C81A, C82A, C83A, C84A, C85A, C86A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1A, C21A, C22A, C23A, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: C21B(0.35) C21A(0.65) C22B(0.35) H22B(0.35) C22A(0.65) H22A(0.65)
 C23B(0.35) H23B(0.35) C23A(0.65) H23A(0.65) C24B(0.35) H24B(0.35) C24A(0.65)
 H24A(0.65) C25B(0.35) H25B(0.35) C25A(0.65) H25A(0.65) C26B(0.35) H26B(0.35)
 C26A(0.65) H26A(0.65) C81B(0.5) C81A(0.5) C82B(0.5) H82B(0.5) C82A(0.5)
 H82A(0.5) C83B(0.5) H83B(0.5) C83A(0.5) H83A(0.5) C84B(0.5) H84B(0.5)
 C84A(0.5) H84A(0.5) C85B(0.5) H85B(0.5) C85A(0.5) H85A(0.5) C86B(0.5)
 H86B(0.5) C86A(0.5) H86A(0.5)
6.a Riding coordinates:
 O1(H1A,H1B), O1A(H1AA,H1AB), O1W(H1WA,H1WB)
6.b Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C9(H9), C13(H13), C14(H14), C18(H18), C19(H19),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), 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), C3A(H3A), C4A(H4A), C8A(H8A),
  C9A(H9A), C13A(H13A), C14A(H14A), C18A(H18A), C19A(H19A), C22B(H22B),
 C22A(H22A), C23B(H23B), C23A(H23A), C24B(H24B), C24A(H24A), C25B(H25B),
 C25A(H25A), C26B(H26B), C26A(H26A), C32A(H32A), C33A(H33A), C34A(H34A),
 C35A(H35A), C36A(H36A), C42A(H42A), C43A(H43A), C44A(H44A), C45A(H45A),
 C46A(H46A), C52A(H52A), C53A(H53A), C54A(H54A), C55A(H55A), C56A(H56A),
 C62A(H62A), C63A(H63A), C64A(H64A), C65A(H65A), C66A(H66A), C72A(H72A),
 C73A(H73A), C74A(H74A), C75A(H75A), C76A(H76A), C82B(H82B), C82A(H82A),
 C83B(H83B), C83A(H83A), C84B(H84B), C84A(H84A), C85B(H85B), C85A(H85A),
 C86B(H86B), C86A(H86A)
;
_shelx_res_checksum              49030
_olex2_submission_special_instructions 'No special instructions were received'