Small molecular neutral microcrystalline iridium(III) complexes as promising molecular oxygen sensors
Ming Li; Baozhan Zheng; Daibing Luo; Huiqin Sun; Ning Wang; Yan Huang; Jun Dai; Dan Xiao; Shi-Jian Su; Zhiyun Lu; Chem.Commun. 51 (2015) 1926–; doi:10.1039/C4cc07252A

data_7116427
_publ_section_title
;
 Small molecular neutral microcrystalline iridium(III) complexes as
 promising molecular oxygen sensors
;
_journal_name_full               Chem.Commun.
_journal_page_first              1926
_journal_paper_doi               10.1039/C4cc07252A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C59 H63 Ir N2 O2 S2, C H2 Cl2'
_chemical_formula_sum            'C60 H65 Cl2 Ir N2 O2 S2'
_chemical_formula_weight         1173.36
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2014-06-04 deposited with the CCDC.
2014-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                103.949(2)
_cell_angle_beta                 93.493(2)
_cell_angle_gamma                103.298(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8835(3)
_cell_length_b                   14.7285(4)
_cell_length_c                   16.0114(4)
_cell_measurement_reflns_used    11371
_cell_measurement_temperature    143.00(10)
_cell_measurement_theta_max      28.7390
_cell_measurement_theta_min      3.2100
_cell_volume                     2847.71(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      143.00(10)
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.5847
_diffrn_measurement_details
;
  1 omega  -12.00   21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3611  -99.0000    0.0000 33

  2 omega  -80.00  -54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3611 -178.0000  -30.0000 26

  3 omega  -24.00   19.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3611  -99.0000   90.0000 43

  4 omega  -48.00    4.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1580  -57.0000   90.0000 52

  5 omega    1.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1580   57.0000    0.0000 87

  6 omega  -50.00    9.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1580  -57.0000 -150.0000 59

  7 omega   -1.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1580   57.0000  -90.0000 76

  8 omega  -25.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1580  -99.0000  150.0000 79
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0194897000
_diffrn_orient_matrix_UB_12      -0.0086039000
_diffrn_orient_matrix_UB_13      -0.0409236000
_diffrn_orient_matrix_UB_21      0.0236268000
_diffrn_orient_matrix_UB_22      -0.0352995000
_diffrn_orient_matrix_UB_23      0.0108565000
_diffrn_orient_matrix_UB_31      -0.0480792000
_diffrn_orient_matrix_UB_32      -0.0361946000
_diffrn_orient_matrix_UB_33      -0.0179737000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25244
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.894
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.553
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.557
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         11636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0432P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10201
_reflns_number_total             11636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc07252a2.cif
_cod_data_source_block           131015_s4_lm
_cod_original_cell_volume        2847.72(13)
_cod_database_code               7116427
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         c12h20n2o3ir2
_shelx_estimated_absorpt_t_max   0.568
_shelx_estimated_absorpt_t_min   0.469
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
Uanis(C57A) = Uanis(C57B)
Uanis(C58A) = Uanis(C58B)
Uanis(C59A) = Uanis(C59B)
3. Others
 Sof(C57B)=Sof(H57D)=Sof(H57E)=Sof(H57F)=Sof(C58B)=Sof(H58D)=Sof(H58E)=
 Sof(H58F)=Sof(C59B)=Sof(H59D)=Sof(H59E)=Sof(H59F)=1-FVAR(1)
 Sof(C57A)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58A)=Sof(H58A)=Sof(H58B)=
 Sof(H58C)=Sof(C59A)=Sof(H59A)=Sof(H59B)=Sof(H59C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C13(H13), C15(H15),
 C17(H17), C19(H19), C29(H29), C35(H35), C36(H36), C37(H37), C38(H38), C42(H42),
  C43(H43), C45(H45), C47(H47), C49(H49), C51(H51)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C),
 C57A(H57A,H57B,H57C), C57B(H57D,H57E,H57F), C58A(H58A,H58B,H58C), C58B(H58D,
 H58E,H58F), C59A(H59A,H59B,H59C), C59B(H59D,H59E,H59F)
;
_shelx_res_checksum              54937