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_7701726
_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         'C70 H48 Ir N4 P, C3 H6 O0.75'
_chemical_formula_sum            'C73 H54 Ir N4 O0.75 P'
_chemical_formula_weight         1222.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.8221(4)
_cell_length_b                   21.8692(4)
_cell_length_c                   25.5085(5)
_cell_measurement_reflns_used    11013
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      27.7090
_cell_measurement_theta_min      3.4690
_cell_volume                     11057.8(4)
_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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega   -4.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8574   77.0000 -180.0000 95

  2 omega  -17.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8574   77.0000   60.0000 100

  3 omega  -41.00   48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8574  -57.0000  -90.0000 89
;
_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      -0.0172284000
_diffrn_orient_matrix_UB_12      -0.0281648000
_diffrn_orient_matrix_UB_13      -0.0032912000
_diffrn_orient_matrix_UB_21      0.0283093000
_diffrn_orient_matrix_UB_22      -0.0120954000
_diffrn_orient_matrix_UB_23      -0.0134982000
_diffrn_orient_matrix_UB_31      0.0135104000
_diffrn_orient_matrix_UB_32      -0.0106568000
_diffrn_orient_matrix_UB_33      0.0240647000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1519
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            62021
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.318
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59898
_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    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4944
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.250
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.128
_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     766
_refine_ls_number_reflns         10817
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0350P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6864
_reflns_number_total             10817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00244h2.cif
_cod_data_source_block           benson57molt
_cod_original_cell_volume        11057.7(4)
_cod_database_code               7701726
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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
2. Rigid bond restraints
 Ir1, C1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Ir1 \\sim C1 \\sim C2 \\sim C3: within 1.2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O1A, C2A, C3S, C4A, C5A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1S, C2S, C3S, C4S, C5S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O1A(0.25) O1S(0.5) C2A(0.25) H2AA(0.25) H2AB(0.25) C2S(0.5)
 H2SA(0.5) H2SB(0.5) C3S(0.75) H3SA(0.5) H3SB(0.5) H3SC(0.25) H3SD(0.25)
 C4A(0.25) H4AA(0.25) H4AB(0.25) C4S(0.5) H4SA(0.5) H4SB(0.5) C5A(0.25)
 H5AA(0.25) H5AB(0.25) C5S(0.5) H5SA(0.5) H5SB(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C3S(H3SC,H3SD), C4A(H4AA,
 H4AB), C4S(H4SA,H4SB), C5A(H5AA,H5AB), C5S(H5SA,H5SB)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), 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)
;
_shelx_res_checksum              43885
_olex2_date_sample_data_collection 2015-12-09
_olex2_submission_special_instructions 'No special instructions were received'