Mono and dinuclear iridium(iii) complexes featuring bis-tridentate coordination and Schiff-base bridging ligands: the beneficial effect of a second metal ion on luminescence.
Puttock, Emma V.; Sil, Amit; Yufit, Dmitry S.; Williams, J. A. Gareth; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10463–10476; doi:10.1039/d0dt01964j

data_7704881
_publ_section_title
;
 Mono and dinuclear iridium(iii) complexes featuring bis-tridentate
 coordination and Schiff-base bridging ligands: the beneficial effect of a
 second metal ion on luminescence.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10463
_journal_page_last               10476
_journal_paper_doi               10.1039/d0dt01964j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C56 H48 Ir2 N10 O2, 2(F6 P), 4(C2 H3 N)'
_chemical_formula_sum            'C64 H60 F12 Ir2 N14 O2 P2'
_chemical_formula_weight         1731.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-08-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r5206)
;
_audit_update_record
;
2020-07-07 deposited with the CCDC.	2020-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                86.983(3)
_cell_angle_beta                 79.538(3)
_cell_angle_gamma                78.218(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7200(11)
_cell_length_b                   14.3155(12)
_cell_length_c                   19.9170(17)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      23.15
_cell_measurement_theta_min      2.41
_cell_volume                     3490.9(5)
_computing_cell_refinement       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_collection       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1680
_diffrn_reflns_av_unetI/netI     0.2280
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            74344
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.108
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.939
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0709 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.8363.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull brownish yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       plate
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.375
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         16016
_refine_ls_number_restraints     914
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0735
_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^)+(0.0840P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8465
_reflns_number_total             16016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01964j2.cif
_cod_data_source_block           Ir2dpyx2L5_16srv305
_cod_depositor_comments
;Adding full bibliography for 7704880--7704885.cif.

 Adding full bibliography for 7704880--7704885.cif.
;
_cod_database_code               7704881
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.649
_computing.bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_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. Restrained distances
 N1S-C1S \\sim N4S-C7S \\sim N3S-C5S \\sim N5S-C9S
 with sigma of 0.005
 C2S-C1S \\sim C8S-C7S \\sim C6S-C5S
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uiso(C12S) = Uiso(C11S)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{N5S, C9S, C10S} sigma for 1-2: 0.02, 1-3: 0.02
{N4S, C7S, C8S} sigma for 1-2: 0.02, 1-3: 0.02
{N3S, C5S, C6S} sigma for 1-2: 0.02, 1-3: 0.02
{N6S, C11S, C12S} sigma for 1-2: 0.005, 1-3: 0.01
as
{N1S, C1S, C2S}
6. Others
 Fixed Sof: N5S(0.7) C9S(0.7) C10S(0.7) H10A(0.7) H10B(0.7) H10C(0.7) N6S(0.3)
 C11S(0.3) C12S(0.3) H12D(0.3) H12E(0.3) H12F(0.3)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C11(H11), C13(H13), C14(H14),
 C15(H15), C16(H16), C22(H22), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
  C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41),
 C42(H42), C48(H48), C53(H53), C54(H54), C55(H55), C56(H56)
7.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C38(H38A,H38B,
 H38C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C2S(H2SA,H2SB,H2SC), C6S(H6SA,
 H6SB,H6SC), C8S(H8SA,H8SB,H8SC), C10S(H10A,H10B,H10C), C12S(H12D,H12E,H12F)
;
_shelx_shelxl_version_number     2014/7