Unprecedented Ir(iii) cationic complexes based on tridentate tetrazolate ligands: synthesis, photophysics and encapsulation in SiO2 nanoparticles
Troya, José; Quesada-Moreno, María Mar; Jiménez, Juan-Ramón; Herrera, Juan Manuel; New Journal of Chemistry 47 (2023) 4577–4585; doi:10.1039/D2NJ06037J

data_7062241
_publ_section_title
;
 Unprecedented Ir(iii) cationic complexes based on tridentate tetrazolate
 ligands: synthesis, photophysics and encapsulation in SiO2 nanoparticles
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4577
_journal_page_last               4585
_journal_paper_doi               10.1039/D2NJ06037J
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C28 H18 Ir N9, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C30 H21 F12 Ir N10 P2'
_chemical_formula_weight         1003.71
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-01-11 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.2258(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6360(5)
_cell_length_b                   11.6774(4)
_cell_length_c                   20.3107(7)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.578
_cell_measurement_theta_min      2.659
_cell_volume                     3233.4(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX4 v2022.1-1 (Bruker, 2022)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker VENTURE'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            74808
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.652
_diffrn_reflns_theta_min         2.296
_exptl_absorpt_coefficient_mu    4.341
_exptl_absorpt_correction_T_max  0.5677
_exptl_absorpt_correction_T_min  0.3402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1021 before and 0.0531 after correction. The Ratio of minimum to maximum transmission is 0.5993. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.062
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.239
_refine_diff_density_max         1.378
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         9938
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0241
_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^)+6.9864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8804
_reflns_number_total             9938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj06037j2.cif
_cod_data_source_block           jmh60
_cod_depositor_comments
'Adding full bibliography for 7062241--7062242.cif.'
_cod_database_code               7062241
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.423
_shelx_estimated_absorpt_t_min   0.321
_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
 P2-F10 \\sim P2-F10A
 with sigma of 0.02
 P2-F9 \\sim P2-F9A
 with sigma of 0.02
 P2-F11 \\sim P2-F11A
 with sigma of 0.02
 P2-F12 \\sim P2-F12A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F12) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F10A)
\\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(F9) \\sim Ueq:
with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(F9A) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F10A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F12) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F10A)
\\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(F9) \\sim Ueq,
Uanis(F12A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(1)
 Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C23(H23), C25(H25),
  C26(H26)
5.b Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              79957
_olex2_submission_special_instructions 'No special instructions were received'