High performance optical oxygen sensors based on iridium complexes exhibiting interchromophore energy shuttling.
Medina-Rodríguez, Santiago; Denisov, Sergey A.; Cudré, Yanouk; Male, Louise; Marín-Suárez, Marta; Fernández-Gutiérrez, Alberto; Fernández-Sánchez, Jorge F; Tron, Arnaud; Jonusauskas, Gediminas; McClenaghan, Nathan D.; Baranoff, Etienne; The Analyst 141 (2016) 3090–3097; doi:10.1039/c6an00497k

data_1543134
_publ_section_title
;
 High performance optical oxygen sensors based on iridium complexes
 exhibiting interchromophore energy shuttling.
;
_journal_issue                   10
_journal_name_full               'The Analyst'
_journal_page_first              3090
_journal_page_last               3097
_journal_paper_doi               10.1039/c6an00497k
_journal_volume                  141
_journal_year                    2016
_chemical_formula_moiety         'C59 H42 Ir N4, F6 P, 4(C H Cl3)'
_chemical_formula_sum            'C63 H46 Cl12 F6 Ir N4 P'
_chemical_formula_weight         1621.61
_chemical_name_common            IrPyr
_chemical_name_systematic        YC49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             14-03-08
_audit_creation_method
;
Rigaku CrystalClear-SM Expert 3.1 b27
;
_audit_update_record
;
2016-02-06 deposited with the CCDC.
2016-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.774(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7764(14)
_cell_length_b                   17.2133(11)
_cell_length_c                   20.4799(14)
_cell_measurement_reflns_used    38423
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     6278.1(7)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
scan:
    Number of images: 165
               Slice: -95.0000 - 70.0000
         Image width: 1.0000
            Exp time: 75.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 18.0000
                 Phi: 150.0000
                 XTD: 49.8860
              2theta: -20.4826
scan:
    Number of images: 99
               Slice: -78.0000 - 21.0000
         Image width: 1.0000
            Exp time: 75.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: -120.0000
                 XTD: 49.8860
              2theta: -20.4826
scan:
    Number of images: 70
               Slice: -32.0000 - 38.0000
         Image width: 1.0000
            Exp time: 75.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 72.0000
                 Phi: -180.0000
                 XTD: 49.8860
              2theta: -20.4826
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
'AFC12 (Right): Kappa 3 circle, Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_orient_matrix_UB_11      0.024281
_diffrn_orient_matrix_UB_12      0.041882
_diffrn_orient_matrix_UB_13      0.028449
_diffrn_orient_matrix_UB_21      0.005075
_diffrn_orient_matrix_UB_22      -0.034503
_diffrn_orient_matrix_UB_23      0.046463
_diffrn_orient_matrix_UB_31      0.054015
_diffrn_orient_matrix_UB_32      0.002860
_diffrn_orient_matrix_UB_33      -0.003776
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37956
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         3.038
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    2.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.707
_refine_diff_density_min         -1.224
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         11690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0723
_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^)+(0.1217P)^2^+21.3892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1897
_refine_ls_wR_factor_ref         0.2063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9165
_reflns_number_total             11690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6an00497k2.cif
_cod_data_source_block           YC-49
_cod_depositor_comments
'Adding full bibliography for 1543134--1543135.cif.'
_cod_database_code               1543134
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C59 H42 Ir1 N4 P1 F6'
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.832
_reflns_odcompleteness_completeness 99.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Ternary CH refined with riding coordinates:
 C601(H601), C701(H701), C801(H801), C901(H901)
2.b Secondary CH2 refined with riding coordinates:
 C102(H10A,H10B), C103(H10C,H10D)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C15(H15), C17(H17), C19(H19), C101(H101), C105(H105),
 C106(H106), C110(H110), C111(H111), C114(H114), C115(H115), C116(H116),
 C118(H118), C119(H119), C32(H32), C33(H33), C34(H34), C35(H35), C39(H39),
 C301(H301), C302(H302), C303(H303), C304(H304), C305(H305), C42(H42), C43(H43),
  C44(H44), C45(H45), C49(H49), C401(H401), C402(H402), C403(H403), C404(H404),
 C405(H405)
2.d Idealised Me refined as rotating group:
 C120(H12A,H12B,H12C)
;
_shelx_res_checksum              48066
_shelx_hkl_checksum              72414
_olex2_submission_special_instructions 'No special instructions were received'