Purine-based Ir(iii) complexes for sensing viscosity of endo-plasmic reticulum with fluorescence lifetime imaging microscopy.
Liu, Xin; Li, Kun; Shi, Lei; Zhang, Hong; Liu, Yan-Hong; Wang, Hao-Yuan; Wang, Nan; Yu, Xiao-Qi; Chemical communications (Cambridge, England) 57 (2021) 2265–2268; doi:10.1039/d0cc07867k

data_7127861
_publ_section_title
;
 Purine-based Ir(iii) complexes for sensing viscosity of endo-plasmic
 reticulum with fluorescence lifetime imaging microscopy.
;
_journal_issue                   18
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2265
_journal_page_last               2268
_journal_paper_doi               10.1039/d0cc07867k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C12 H9 Cl N4'
_chemical_formula_sum            'C12 H9 Cl N4'
_chemical_formula_weight         244.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2020-07-04 deposited with the CCDC.	2021-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.083(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9944(5)
_cell_length_b                   11.3189(5)
_cell_length_c                   14.3507(7)
_cell_measurement_reflns_used    2485
_cell_measurement_temperature    297.5(2)
_cell_measurement_theta_max      71.3440
_cell_measurement_theta_min      4.9910
_cell_volume                     1124.84(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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      air
_diffrn_ambient_temperature      297.5(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.952
_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   -105.00 -17.00   1.00    1.00    --  -36.29 -38.00  60.00   88
  2  \w     23.00  90.00   1.00    1.00    --   36.29-125.00 120.00   67
  3  \w    -33.00 106.00   1.00    1.00    --   36.29   0.00-180.00  139
  4  \w     23.00  90.00   1.00    1.00    --   36.29-125.00 -90.00   67
  5  \w    -33.00 106.00   1.00    1.00    --   36.29   0.00-180.00  139
  6  \w     39.00 133.00   1.00    2.24    --  106.21 -77.00 -90.00   94
  7  \w    100.00 176.00   1.00    2.24    --  106.21 111.00   0.00   76
  8  \w     39.00 124.00   1.00    2.24    --  106.21 -61.00 -60.00   85
  9  \w    100.00 176.00   1.00    2.24    --  106.21 111.00-120.00   76
 10  \w     57.00 150.00   1.00    2.24    --  106.21 178.00-180.00   93
 11  \w     88.00 173.00   1.00    2.24    --  106.21  61.00 -60.00   85
 12  \w   -104.00 -20.00   1.00    1.00    --  -36.29 -57.00 -30.00   84
 13  \w   -104.00 -20.00   1.00    1.00    --  -36.29 -57.00-120.00   84
 14  \w     10.00 104.00   1.00    1.00    --   36.29  77.00-180.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0115711000
_diffrn_orient_matrix_UB_12      -0.1013747000
_diffrn_orient_matrix_UB_13      0.0721746000
_diffrn_orient_matrix_UB_21      0.1302956000
_diffrn_orient_matrix_UB_22      0.0765699000
_diffrn_orient_matrix_UB_23      0.0716125000
_diffrn_orient_matrix_UB_31      -0.1800617000
_diffrn_orient_matrix_UB_32      0.0487698000
_diffrn_orient_matrix_UB_33      0.0375998000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5976
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.775
_diffrn_reflns_theta_min         4.996
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       needle
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1377P)^2^+0.0123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1887
_refine_ls_wR_factor_ref         0.1996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1752
_reflns_number_total             2102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07867k2.cif
_cod_data_source_block           yxq-lx-3
_cod_depositor_comments
'Adding full bibliography for 7127860--7127861.cif.'
_cod_database_code               7127861
_reflns_odcompleteness_completeness 97.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C009(H009), C00C(H00C), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G)
2.b Idealised Me refined as rotating group:
 C00H(H00A,H00B,H00H)
;
_shelx_res_checksum              53991
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2019-09-10
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.751
_oxdiff_exptl_absorpt_empirical_full_min 0.539