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_7062242
_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         'C26 H14 Ir N12, F6 P, 4(C2 H3 N)'
_chemical_formula_sum            'C34 H26 F6 Ir N16 P'
_chemical_formula_weight         995.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2019-12-18
_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                 120.168(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.841(3)
_cell_length_b                   12.3097(19)
_cell_length_c                   18.522(4)
_cell_measurement_reflns_used    9430
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.396
_cell_measurement_theta_min      2.544
_cell_volume                     3713.9(12)
_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 0.995
_diffrn_measurement_device_type  'Bruker VENTURE'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55479
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.422
_diffrn_reflns_theta_min         2.501
_exptl_absorpt_coefficient_mu    3.720
_exptl_absorpt_correction_T_max  0.5192
_exptl_absorpt_correction_T_min  0.4624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0598 before and 0.0513 after correction. The Ratio of minimum to maximum transmission is 0.8906. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'metallic orangish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.145
_refine_diff_density_max         0.606
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0164
_refine_ls_R_factor_gt           0.0151
_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^)+(0.0195P)^2^+4.1173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0386
_refine_ls_wR_factor_ref         0.0390
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4458
_reflns_number_total             4647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj06037j2.cif
_cod_data_source_block           jt4f2_new
_cod_depositor_comments
'Adding full bibliography for 7062241--7062242.cif.'
_cod_original_cell_volume        3713.9(11)
_cod_database_code               7062242
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.615
_shelx_estimated_absorpt_t_min   0.398
_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.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C11(H11), C6(H6), C2(H2), C8(H8), C3(H3)
2.b Idealised Me refined as rotating group:
 C1S(H1Sa,H1Sb,H1Sc), C3S(H3Sa,H3Sb,H3Sc)
;
_shelx_res_checksum              74744
_olex2_submission_special_instructions 'No special instructions were received'