A novel iridium(iii) complex for sensitive HSA phosphorescence staining in proteome research.
Wang, Yi; Huang, Huaiyi; Chen, Ge; Chen, Haijie; Xu, Tingting; Tang, Qian; Zhu, Hailiang; Zhang, Qianling; Zhang, Pingyu; Chemical communications (Cambridge, England) 54 (2018) 3282–3285; doi:10.1039/c8cc01597j

data_7121352
_publ_section_title
;
 A novel iridium(iii) complex for sensitive HSA phosphorescence staining
 in proteome research.
;
_journal_issue                   26
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3282
_journal_page_last               3285
_journal_paper_doi               10.1039/c8cc01597j
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C34 H25 Ir N4 S, 2(C2 H6 O S), 0.5(C2 H6 O)'
_chemical_formula_sum            'C39 H40 Ir N4 O2.5 S3'
_chemical_formula_weight         893.13
_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
_audit_creation_date             2015-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-06-29 deposited with the CCDC.
2018-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                97.9685(12)
_cell_angle_beta                 95.6471(11)
_cell_angle_gamma                101.1031(14)
_cell_formula_units_Z            2
_cell_length_a                   12.17572(19)
_cell_length_b                   12.5686(2)
_cell_length_c                   12.97302(16)
_cell_measurement_reflns_used    27049
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      36.8830
_cell_measurement_theta_min      3.3280
_cell_volume                     1913.26(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      6.00  99.00   1.00    3.75    --   29.88  57.00  60.00   93
  2  \w     14.00  94.00   1.00    3.75    --   29.88  38.00 150.00   80
  3  \w     11.00 102.00   1.00    3.75    --   29.88  57.00 -30.00   91
  4  \w      2.00  91.00   1.00    3.75    --   29.88  57.00-120.00   89
  5  \w    -41.00  44.00   1.00    3.75    --   29.88 -38.00  60.00   85
  6  \w    -44.00  49.00   1.00    3.75    --   29.88 -38.00 -30.00   93
  7  \w      1.00  28.00   1.00    3.75    --  -30.82-131.00-145.77   27
  8  \w     36.00  95.00   1.00    3.75    --   29.88-178.00   0.00   59
  9  \w     83.00 117.00   1.00    3.75    --   29.88-178.00  90.00   34
 10  \w    -49.00  42.00   1.00    3.75    --  -30.82  38.00-150.00   91
 11  \w    -86.00 -42.00   1.00    3.75    --  -30.82 123.00-169.00   44
 12  \w   -109.00 -63.00   1.00    3.75    --  -30.82 158.00   6.39   46
 13  \w     48.00  74.00   1.00    3.75    --   29.88-178.00  90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0547639000
_diffrn_orient_matrix_UB_12      0.0240750000
_diffrn_orient_matrix_UB_13      -0.0099852000
_diffrn_orient_matrix_UB_21      0.0175862000
_diffrn_orient_matrix_UB_22      -0.0500668000
_diffrn_orient_matrix_UB_23      0.0039404000
_diffrn_orient_matrix_UB_31      -0.0165954000
_diffrn_orient_matrix_UB_32      -0.0175955000
_diffrn_orient_matrix_UB_33      -0.0546265000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            64436
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         37.659
_diffrn_reflns_theta_min         2.637
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.693
_exptl_absorpt_correction_T_max  0.454
_exptl_absorpt_correction_T_min  0.221
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       block
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.828
_exptl_crystal_size_mid          0.388
_exptl_crystal_size_min          0.325
_refine_diff_density_max         4.011
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         19457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+2.1735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17022
_reflns_number_total             19457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01597j3.cif
_cod_data_source_block           pz2
_cod_depositor_comments          'Adding full bibliography for 7121352.cif.'
_cod_original_cell_volume        1913.27(5)
_cod_original_formula_sum        'C39 H40 Ir N4 O2.50 S3'
_cod_database_code               7121352
_chemical_oxdiff_formula         'C40 H40 N3 O2 S3 Ir'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
One of the DMSO molecules was modeled as disordered over two positions.
The two positions of disordered DMSO shared the same methyl positions.  
The occupancy of the disordered components was fixed at 60:40. 
The hydrogens of the OH on the partially occupied ethanol 
(modeled at 50% occupancy) was placed at a calculated position. 
The minor disordered component of the DMSO and the ethanol were 
refined isotropically.

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, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) H42A(0.6) H42B(0.6)
 H42C(0.6) H42D(0.4) H42E(0.4) H42F(0.4) H40A(0.6) H40B(0.6) H40C(0.6)
 H40D(0.4) H40E(0.4) H40F(0.4) S41(0.6) S41A(0.4) C47(0.5) H47A(0.5) H47B(0.5)
 O41(0.6) O41A(0.4) O48(0.5) H48(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B)
3.b Me refined with riding coordinates:
 C46(H46A,H46B,H46C), C42(H42A,H42B,H42C), C42(H42D,H42E,H42F), C40(H40A,H40B,
 H40C), C40(H40D,H40E,H40F)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16),
 C19(H19), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C29(H29),
  C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), C38(H38)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C45(H45A,H45B,H45C), C43(H43A,H43B,H43C)
3.e Idealised tetrahedral OH refined as rotating group:
 O48(H48)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.093
_oxdiff_exptl_absorpt_empirical_full_min 0.921