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_1543135
_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         'C76 H52 Ir N4, F6 P, 1.25(C H2 Cl2)'
_chemical_formula_sum            'C77.25 H54.5 Cl2.5 F6 Ir N4 P'
_chemical_formula_weight         1464.54
_chemical_name_systematic        IrbisPyr
_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     direct
_audit_creation_date             14-09-21
_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                67.2098(19)
_cell_angle_beta                 75.538(2)
_cell_angle_gamma                78.319(2)
_cell_formula_units_Z            4
_cell_length_a                   13.1487(9)
_cell_length_b                   23.0231(16)
_cell_length_c                   23.3516(16)
_cell_measurement_reflns_used    99839
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.1
_cell_volume                     6266.3(8)
_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                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support MiTeGen
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1073
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            95074
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.955
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    2.331
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.545
_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    1.552
_exptl_crystal_description       lath
_exptl_crystal_F_000             2938
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.049
_refine_diff_density_min         -2.224
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1713
_refine_ls_number_reflns         23701
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+14.3260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1815
_refine_ls_wR_factor_ref         0.1939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19175
_reflns_number_total             23701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6an00497k2.cif
_cod_data_source_block           Ir-bis_Pyr
_cod_depositor_comments
'Adding full bibliography for 1543134--1543135.cif.'
_cod_original_formula_sum        'C77.25 H54.50 Cl2.50 F6 Ir N4 P'
_cod_database_code               1543135
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.616
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl94-C902
 1.75 with sigma of 0.02
 Cl93-C902
 1.75 with sigma of 0.02
 Cl5'-C93'
 1.75 with sigma of 0.02
 Cl6'-C93'
 1.75 with sigma of 0.02
 C508-C507 = C509-C508 = C510-C509 = C511-C510 = C512-C511 = C513-C512 = C513-
 C508 = C514-C512 = C515-C514 = C516-C515 = C517-C516 = C517-C513 = C518-C517 =
 C519-C518 = C519-C507
 1.39 with sigma of 0.02
3. Rigid bond restraints
 C504, C505, C506, C507, C508, C509, C510, C511, C512, C513, C514, C515, C516,
 C517, C518, C519
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P902, F911
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C93', Cl5', Cl6'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(C20')=Sof(H20A)=Sof(H20B)=Sof(C21')=Sof(H21A)=Sof(H21B)=1-FVAR(1)
 Sof(C520)=Sof(H52A)=Sof(H52B)=Sof(C521)=Sof(H52C)=Sof(H52D)=FVAR(1)
 Sof(C93')=Sof(H93A)=Sof(H93B)=Sof(Cl5')=Sof(Cl6')=1-FVAR(2)
 Sof(C903)=Sof(H90E)=Sof(H90F)=Sof(Cl5)=Sof(Cl6)=FVAR(2)
 Fixed Sof: C902(0.5) H90C(0.5) H90D(0.5) Cl93(0.5) Cl94(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C102(H10A,H10B), C103(H10C,H10D), C120(H12A,H12B), C121(H12C,H12D), C502(H50A,
 H50B), C503(H50C,H50D), C520(H52A,H52B), C521(H52C,H52D), C20'(H20A,H20B),
 C21'(H21A,H21B), C901(H90A,H90B), C902(H90C,H90D), C903(H90E,H90F), C93'(H93A,
 H93B)
5.b 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), C123(H123), C124(H124), C128(H128), C129(H129),
 C132(H132), C133(H133), C134(H134), C136(H136), C137(H137), 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), C52(H52), C54(H54), C55(H55),
 C57(H57), C59(H59), C501(H501), C505(H505), C506(H506), C510(H510), C511(H511),
  C514(H514), C515(H515), C516(H516), C518(H518), C519(H519), C523(H523),
 C524(H524), C528(H528), C529(H529), C532(H532), C533(H533), C534(H534),
 C536(H536), C537(H537), C72(H72), C73(H73), C74(H74), C75(H75), C79(H79),
 C701(H701), C702(H702), C703(H703), C704(H704), C705(H705), C82(H82), C83(H83),
  C84(H84), C85(H85), C89(H89), C801(H801), C802(H802), C803(H803), C804(H804),
 C805(H805)
;
_shelx_res_checksum              46878
_shelx_hkl_checksum              51869
_olex2_submission_special_instructions 'No special instructions were received'