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_7116428
_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         'C31 H23 Ir N2 O2 S2, 0.25(C H4 O)'
_chemical_formula_sum            'C31.25 H24 Ir N2 O2.25 S2'
_chemical_formula_weight         719.84
_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             2014-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2014-06-04 deposited with the CCDC.
2014-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                107.775(3)
_cell_angle_beta                 99.052(2)
_cell_angle_gamma                117.763(3)
_cell_formula_units_Z            8
_cell_length_a                   18.4383(5)
_cell_length_b                   18.6855(6)
_cell_length_c                   19.9281(6)
_cell_measurement_reflns_used    15404
_cell_measurement_temperature    142.95(10)
_cell_measurement_theta_max      28.8220
_cell_measurement_theta_min      3.1820
_cell_volume                     5407.5(4)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      142.95(10)
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -71.00    3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5174  121.0000 -115.0000 74

  2 omega  -18.00   19.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5174  -99.0000  120.0000 37

  3 omega   -5.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2361  -99.0000   60.0000 50

  4 omega    2.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2361   57.0000 -120.0000 86

  5 omega   -5.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2361   38.0000  150.0000 96

  6 omega  -48.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2361  -38.0000  -30.0000 83
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0167780000
_diffrn_orient_matrix_UB_12      0.0350441000
_diffrn_orient_matrix_UB_13      0.0364943000
_diffrn_orient_matrix_UB_21      -0.0088688000
_diffrn_orient_matrix_UB_22      -0.0311647000
_diffrn_orient_matrix_UB_23      0.0157361000
_diffrn_orient_matrix_UB_31      0.0424636000
_diffrn_orient_matrix_UB_32      0.0081314000
_diffrn_orient_matrix_UB_33      0.0044379000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44827
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.040
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61020
_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    1.768
_exptl_crystal_F_000             2818
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         3.400
_refine_diff_density_min         -2.196
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1396
_refine_ls_number_reflns         22073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0375P)^2^+15.3766P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17545
_reflns_number_total             22073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc07252a2.cif
_cod_data_source_block           140513_s1_lm_m
_cod_original_cell_volume        5407.5(3)
_cod_database_code               7116428
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         c12h12n3o2s1ir1
_shelx_estimated_absorpt_t_max   0.308
_shelx_estimated_absorpt_t_min   0.267
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C23(H23), C24(H24), C25(H25), C26(H26),
  C28(H28), C64(H64), C65(H65), C66(H66), C67(H67), C72(H72), C73(H73),
 C74(H74), C75(H75), C77(H77), C78(H78), C79(H79), C80(H80), C85(H85), C86(H86),
  C87(H87), C88(H88), C90(H90), C95(H95), C96(H96), C97(H97), C98(H98),
 C103(H103), C104(H104), C105(H105), C106(H106), C108(H108), C109(H109),
 C110(H110), C111(H111), C116(H116), C117(H117), C118(H118), C119(H119),
 C121(H121), C33(H33), C34(H34), C35(H35), C36(H36), C41(H41), C42(H42),
 C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C53(H53), C54(H54),
  C55(H55), C56(H56), C59(H59)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C92(H92A,H92B,H92C), C93(H93A,H93B,
 H93C), C123(H12A,H12B,H12C), C124(H12D,H12E,H12F), C61(H61A,H61B,H61C),
 C62(H62A,H62B,H62C), C125(H12G,H12H,H12I)
;
_shelx_res_checksum              65692