#------------------------------------------------------------------------------
#$Date: 2023-03-04 20:36:15 +0200 (Sat, 04 Mar 2023) $
#$Revision: 281538 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/22/7062242.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7062242
loop_
_publ_author_name
'Troya, José'
'Quesada-Moreno, María Mar'
'Jiménez, Juan-Ramón'
'Herrera, Juan Manuel'
_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 λ/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/[σ²(Fo²)+(0.0195P)²+4.1173P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.0000 0.02404(2) 0.7500 0.00944(3) Uani 1 2 d S T P . .
P2 P 0.2500 -0.2500 1.0000 0.02495(15) Uani 1 2 d S T P . .
F4 F 0.15190(8) -0.26140(12) 0.94811(8) 0.0344(3) Uani 1 1 d . . . . .
F5 F 0.25420(8) -0.29117(11) 0.91991(7) 0.0318(3) Uani 1 1 d . . . . .
F6 F 0.24210(8) -0.12691(11) 0.96816(8) 0.0334(3) Uani 1 1 d . . . . .
N2 N -0.07487(9) 0.02788(11) 0.62665(9) 0.0117(3) Uani 1 1 d . . . . .
N3 N 0.08122(9) 0.14274(11) 0.76338(8) 0.0140(3) Uani 1 1 d . . . . .
N1 N -0.05455(8) -0.09485(11) 0.78599(8) 0.0123(3) Uani 1 1 d . . . . .
N4 N -0.09251(10) 0.21425(12) 0.78428(9) 0.0195(3) Uani 1 1 d . . . . .
C7 C -0.05646(10) -0.03928(13) 0.58123(10) 0.0125(3) Uani 1 1 d . . . . .
C9 C -0.10185(11) -0.03934(14) 0.49396(10) 0.0153(3) Uani 1 1 d . . . . .
C1 C 0.12035(10) -0.15668(15) 0.75893(11) 0.0173(3) Uani 1 1 d . . . . .
H1 H 0.1495 -0.1501 0.8180 0.021 Uiso 1 1 calc R . . . .
N6 N -0.18639(10) 0.24553(14) 0.65288(10) 0.0245(3) Uani 1 1 d . . . . .
C10 C -0.16648(11) 0.03674(15) 0.45620(11) 0.0186(3) Uani 1 1 d . . . . .
H10 H -0.1986 0.0402 0.3970 0.022 Uiso 1 1 calc R . . . .
C13 C -0.13931(10) 0.16390(14) 0.65627(10) 0.0162(3) Uani 1 1 d . . . . .
N5 N -0.15584(11) 0.27516(14) 0.73391(10) 0.0266(4) Uani 1 1 d . . . . .
C11 C -0.18382(11) 0.10631(15) 0.50400(11) 0.0189(3) Uani 1 1 d . . . . .
H11 H -0.2271 0.1577 0.4781 0.023 Uiso 1 1 calc R . . . .
C2S C 0.29866(15) -0.01538(17) 0.81644(16) 0.0298(4) Uani 1 1 d . . . . .
C5 C 0.01301(10) -0.10671(13) 0.62817(10) 0.0128(3) Uani 1 1 d . . . . .
N1S N 0.24803(15) 0.03022(16) 0.76106(16) 0.0408(5) Uani 1 1 d . . . . .
C12 C -0.13633(10) 0.09981(14) 0.59148(10) 0.0152(3) Uani 1 1 d . . . . .
C4 C 0.03656(10) -0.17913(14) 0.58578(11) 0.0166(3) Uani 1 1 d . . . . .
C6 C -0.01126(11) -0.18139(14) 0.49585(11) 0.0191(3) Uani 1 1 d . . . . .
H6 H 0.0035 -0.2310 0.4663 0.023 Uiso 1 1 calc R . . . .
C2 C 0.14775(12) -0.23159(16) 0.72081(12) 0.0231(4) Uani 1 1 d . . . . .
H2 H 0.1948 -0.2749 0.7545 0.028 Uiso 1 1 calc R . . . .
C8 C -0.07681(11) -0.11471(15) 0.45190(11) 0.0186(3) Uani 1 1 d . . . . .
H8 H -0.1064 -0.1181 0.3926 0.022 Uiso 1 1 calc R . . . .
C3 C 0.10715(12) -0.24280(15) 0.63544(12) 0.0220(4) Uani 1 1 d . . . . .
H3 H 0.1263 -0.2928 0.6100 0.026 Uiso 1 1 calc R . . . .
C1S C 0.36341(16) -0.0739(2) 0.88756(15) 0.0407(5) Uani 1 1 d . . . . .
H1SA H 0.3750 -0.0376 0.9394 0.061 Uiso 1 1 calc GR . . . .
H1SB H 0.4132 -0.0748 0.8833 0.061 Uiso 1 1 calc GR . . . .
H1SC H 0.3455 -0.1486 0.8877 0.061 Uiso 1 1 calc GR . . . .
C4S C 0.40313(18) 0.0574(3) 1.1002(2) 0.0535(8) Uani 1 1 d . . . . .
C3S C 0.3905(2) -0.0076(3) 1.1585(2) 0.0542(7) Uani 1 1 d . . . . .
H3SA H 0.3341 -0.0354 1.1303 0.081 Uiso 1 1 calc GR . . . .
H3SB H 0.3998 0.0375 1.2061 0.081 Uiso 1 1 calc GR . . . .
H3SC H 0.4291 -0.0687 1.1784 0.081 Uiso 1 1 calc GR . . . .
N2S N 0.4112(2) 0.1091(3) 1.0538(2) 0.0828(11) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ir1 N2 177.28(8) . 2_556 ?
N2 Ir1 N3 100.25(5) . . ?
N2 Ir1 N3 77.77(6) 2_556 . ?
N2 Ir1 N3 100.25(5) 2_556 2_556 ?
N2 Ir1 N3 77.77(6) . 2_556 ?
N2 Ir1 N1 80.12(6) . 2_556 ?
N2 Ir1 N1 80.12(6) 2_556 . ?
N2 Ir1 N1 101.83(5) . . ?
N2 Ir1 N1 101.83(5) 2_556 2_556 ?
N3 Ir1 N3 88.44(8) . 2_556 ?
N3 Ir1 N1 94.68(5) 2_556 . ?
N3 Ir1 N1 157.87(5) . . ?
N3 Ir1 N1 157.87(5) 2_556 2_556 ?
N3 Ir1 N1 94.68(5) . 2_556 ?
N1 Ir1 N1 90.63(7) 2_556 . ?
F4 P2 F4 180.0 7_547 . ?
F4 P2 F5 89.76(7) 7_547 7_547 ?
F4 P2 F5 90.24(6) . 7_547 ?
F4 P2 F5 90.24(6) 7_547 . ?
F4 P2 F5 89.76(7) . . ?
F4 P2 F6 89.79(7) 7_547 7_547 ?
F4 P2 F6 89.79(7) . . ?
F4 P2 F6 90.21(7) . 7_547 ?
F4 P2 F6 90.22(7) 7_547 . ?
F5 P2 F5 180.00(9) . 7_547 ?
F6 P2 F5 89.83(7) . . ?
F6 P2 F5 90.17(7) 7_547 . ?
F6 P2 F5 90.17(7) . 7_547 ?
F6 P2 F5 89.83(7) 7_547 7_547 ?
F6 P2 F6 180.0 . 7_547 ?
C7 N2 Ir1 116.52(11) . . ?
C12 N2 Ir1 120.96(11) . . ?
C12 N2 C7 122.34(15) . . ?
N4 N3 Ir1 138.61(11) 2_556 . ?
N4 N3 C13 106.81(14) 2_556 2_556 ?
C13 N3 Ir1 114.40(11) 2_556 . ?
C1 N1 Ir1 131.04(11) 2_556 . ?
C1 N1 C5 118.02(14) 2_556 2_556 ?
C5 N1 Ir1 110.94(10) 2_556 . ?
N5 N4 N3 107.15(14) . 2_556 ?
N2 C7 C9 121.60(16) . . ?
N2 C7 C5 115.16(14) . . ?
C9 C7 C5 123.22(15) . . ?
C7 C9 C10 116.52(16) . . ?
C7 C9 C8 116.81(16) . . ?
C10 C9 C8 126.64(16) . . ?
N1 C1 C2 121.48(16) 2_556 . ?
C13 N6 N5 104.47(15) . . ?
C11 C10 C9 121.04(16) . . ?
N3 C13 C12 117.02(15) 2_556 . ?
N6 C13 N3 110.51(15) . 2_556 ?
N6 C13 C12 132.38(16) . . ?
N4 N5 N6 111.05(15) . . ?
C10 C11 C12 118.97(16) . . ?
N1S C2S C1S 179.8(3) . . ?
N1 C5 C7 117.23(14) 2_556 . ?
N1 C5 C4 123.82(15) 2_556 . ?
C4 C5 C7 118.93(15) . . ?
N2 C12 C13 109.79(14) . . ?
N2 C12 C11 119.51(16) . . ?
C11 C12 C13 130.65(16) . . ?
C5 C4 C6 118.05(16) . . ?
C5 C4 C3 116.60(16) . . ?
C3 C4 C6 125.33(16) . . ?
C8 C6 C4 122.13(15) . . ?
C3 C2 C1 120.69(17) . . ?
C6 C8 C9 120.83(15) . . ?
C2 C3 C4 119.38(16) . . ?
N2S C4S C3S 178.4(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 N2 1.9933(15) . ?
Ir1 N2 1.9933(15) 2_556 ?
Ir1 N3 2.0388(14) 2_556 ?
Ir1 N3 2.0388(14) . ?
Ir1 N1 2.0812(13) 2_556 ?
Ir1 N1 2.0812(13) . ?
P2 F4 1.6044(13) 7_547 ?
P2 F4 1.6045(13) . ?
P2 F5 1.6068(12) 7_547 ?
P2 F5 1.6068(12) . ?
P2 F6 1.6055(13) . ?
P2 F6 1.6055(13) 7_547 ?
N2 C7 1.343(2) . ?
N2 C12 1.338(2) . ?
N3 N4 1.3372(19) 2_556 ?
N3 C13 1.358(2) 2_556 ?
N1 C1 1.331(2) 2_556 ?
N1 C5 1.382(2) 2_556 ?
N4 N3 1.3372(19) 2_556 ?
N4 N5 1.318(2) . ?
C7 C9 1.398(2) . ?
C7 C5 1.419(2) . ?
C9 C10 1.412(3) . ?
C9 C8 1.435(2) . ?
C1 N1 1.331(2) 2_556 ?
C1 C2 1.408(2) . ?
N6 C13 1.321(2) . ?
N6 N5 1.360(2) . ?
C10 C11 1.384(3) . ?
C13 N3 1.358(2) 2_556 ?
C13 C12 1.461(2) . ?
C11 C12 1.405(2) . ?
C2S N1S 1.137(3) . ?
C2S C1S 1.459(3) . ?
C5 N1 1.382(2) 2_556 ?
C5 C4 1.400(2) . ?
C4 C6 1.442(2) . ?
C4 C3 1.414(2) . ?
C6 C8 1.361(3) . ?
C2 C3 1.374(3) . ?
C4S C3S 1.455(5) . ?
C4S N2S 1.140(5) . ?
