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_7704885
_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
'2(C64 H64 Ir2 N10 O2), 3(F6 P), C H4 O, 6(C2 H3 N)'
_chemical_formula_sum            'C141 H150 F18 Ir4 N26 O5 P3'
_chemical_formula_weight         3492.57
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2020-07-07 deposited with the CCDC.	2020-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                75.235(3)
_cell_angle_beta                 76.582(3)
_cell_angle_gamma                87.493(3)
_cell_formula_units_Z            1
_cell_length_a                   12.2674(11)
_cell_length_b                   16.3422(15)
_cell_length_c                   21.227(2)
_cell_measurement_reflns_used    9442
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      31.46
_cell_measurement_theta_min      2.43
_cell_volume                     4002.1(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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    '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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w-scan
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            83046
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         2.120
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.422
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.0667 before and 0.0509 after correction. 
The Ratio of minimum to maximum transmission is 0.8352. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       prism
_exptl_crystal_F_000             1733
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         4.907
_refine_diff_density_min         -3.051
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         21245
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0230P)^2^+45.6800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16817
_reflns_number_total             21245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01964j2.cif
_cod_data_source_block           Ir2dpyx2L6_16srv324
_cod_depositor_comments
;Adding full bibliography for 7704880--7704885.cif.

 Adding full bibliography for 7704880--7704885.cif.
;
_cod_original_cell_volume        4002.2(6)
_cod_database_code               7704885
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.611
_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, All O(H) groups
2. Restrained distances
 P2-F6A \\sim P2-F4 \\sim P2-F4A \\sim P2-F8 \\sim P2-F8A \\sim P2-F9 \\sim
P2-F9A \\sim P2-F6
 with sigma of 0.005
 N1S-C2S \\sim N2S-C4S \\sim N3S-C6S \\sim N4S-C8S
 with sigma of 0.005
 C3S-C2S \\sim C5S-C4S \\sim C7S-C6S \\sim C9S-C8S
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.005
Uanis(C5S) \\sim Ueq, Uanis(C4S) \\sim Ueq, Uanis(N2S) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C17A(0.5) H17D(0.5)
 H17E(0.5) H17F(0.5) C26(0.6) H26A(0.6) H26B(0.6) H26C(0.6) C26A(0.4) H26D(0.4)
 H26E(0.4) H26F(0.4) C27(0.6) H27A(0.6) H27B(0.6) H27C(0.6) C27A(0.4) H27D(0.4)
 H27E(0.4) H27F(0.4) C28(0.6) H28A(0.6) H28B(0.6) H28C(0.6) C28A(0.4) H28D(0.4)
 H28E(0.4) H28F(0.4) F4(0.5) F4A(0.5) F6(0.5) F6A(0.5) F8(0.5) F8A(0.5) F9(0.5)
 F9A(0.5) O1S(0.5) H1S(0.5) C10S(0.5) H10D(0.5) H10E(0.5) H10F(0.5) N1S(0.5)
 C2S(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) H3SC(0.5) N4S(0.5) C8S(0.5) C9S(0.5)
 H9SA(0.5) H9SB(0.5) H9SC(0.5)
5.a Riding coordinates:
 C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), O1S(H1S), C10S(H10D,H10E,H10F),
 C3S(H3SA,H3SB,H3SC), C5S(H5SA,H5SB,H5SC), C7S(H7SA,H7SB,H7SC), C9S(H9SA,H9SB,
 H9SC)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C11(H11), C14(H14), C16(H16), C18(H18), C21(H21),
 C22(H22), C24(H24), C29(H29), C30(H30), C31(H31), C32(H32), C38(H38), C43(H43),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
 C56(H56), C61(H61), C62(H62), C63(H63), C64(H64)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C26(H26A,H26B,H26C), C26A(H26D,H26E,H26F), C27(H27A,H27B,H27C), C27A(H27D,H27E,
 H27F), C28(H28A,H28B,H28C), C28A(H28D,H28E,H28F), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C)
;