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_7116426
_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         'C39 H39 Ir N2 O2 S2'
_chemical_formula_sum            'C39 H39 Ir N2 O2 S2'
_chemical_formula_weight         824.04
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-04-23
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.4876(4)
_cell_length_b                   18.3802(6)
_cell_length_c                   27.8072(9)
_cell_measurement_reflns_used    10006
_cell_measurement_temperature    142.95(10)
_cell_measurement_theta_max      28.7920
_cell_measurement_theta_min      3.2070
_cell_volume                     6893.5(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_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0311494000
_diffrn_orient_matrix_UB_12      -0.0287924000
_diffrn_orient_matrix_UB_13      -0.0077648000
_diffrn_orient_matrix_UB_21      0.0345951000
_diffrn_orient_matrix_UB_22      -0.0088533000
_diffrn_orient_matrix_UB_23      -0.0183228000
_diffrn_orient_matrix_UB_31      0.0244986000
_diffrn_orient_matrix_UB_32      -0.0240977000
_diffrn_orient_matrix_UB_33      0.0159604000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            39733
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.930
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67461
_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    1.588
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.179
_refine_diff_density_min         -3.024
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0271P)^2^+57.0117P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5382
_reflns_number_total             7034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc07252a2.cif
_cod_data_source_block           140421_s1_lm_m
_cod_database_code               7116426
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         chnomg
_shelx_estimated_absorpt_t_max   0.432
_shelx_estimated_absorpt_t_min   0.295
_reflns_odcompleteness_completeness 99.73
_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:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C12(H12), C13(H13), C20(H20),
 C21(H21), C22(H22), C23(H23), C27(H27), C29(H29), C30(H30), C36(H36)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C)
;
_shelx_res_checksum              26027