Synthesis and characterization of <sup>15</sup>N-labeled tetranuclear Ir complexes <i>via</i> Li<sub>2</sub>C<sup>15</sup>N<sub>2</sub>.
Yan, Xuechao; Ji, Shu-Xiao; Zhang, Shengyuan; Wang, Qianru; Guo, Jianping; Chen, Ping; Xi, Zhenfeng; Wei, Junnian; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6246–6251; doi:10.1039/d5dt00644a

data_7718378
_publ_section_title
;
 Synthesis and characterization of <sup>15</sup>N-labeled tetranuclear Ir
 complexes <i>via</i> Li<sub>2</sub>C<sup>15</sup>N<sub>2</sub>.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6246
_journal_page_last               6251
_journal_paper_doi               10.1039/d5dt00644a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C44 H60 Ir4 N8, C32 H12 B F24'
_chemical_formula_sum            'C76 H72 B F24 Ir4 N8'
_chemical_formula_weight         2333.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-12-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-12-21 deposited with the CCDC.	2025-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3731(2)
_cell_length_b                   19.4020(2)
_cell_length_c                   20.8027(2)
_cell_measurement_reflns_used    95418
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      30.1760
_cell_measurement_theta_min      2.3810
_cell_volume                     7819.25(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     53.00  79.00   0.50    4.13    --   -5.70  82.00  60.00   52
  2  \w     57.00  83.00   0.50    4.13    --   -5.70  77.00 -90.00   52
  3  \w    -43.00  27.00   0.50    4.13    --   -5.70  82.00-120.00  140
  4  \w     58.00  84.00   0.50    4.13    --   -5.70  82.00-120.00   52
  5  \w    -43.00  34.00   0.50    4.13    --   -5.70  82.00  60.00  154
  6  \w    -43.00  57.00   0.50    4.13    --   -5.70  82.00 -30.00  200
  7  \w    -43.00  83.00   0.50    4.13    --   -5.70  82.00-180.00  252
  8  \w    -43.00  82.00   0.50    4.13    --   -5.70  82.00 150.00  250
  9  \w    -41.00  25.00   0.50    4.13    --   -5.70  77.00 -90.00  132
 10  \w    -17.00  91.00   0.50    4.13    --    5.70  57.00 -60.00  216
 11  \w     11.00  43.00   0.50    4.13    --    5.70 -80.00  45.59   64
 12  \w    -70.00 -11.00   0.50    4.13    --    5.70 -80.00  45.59  118
 13  \w    -32.00  88.00   0.50    4.13    --    5.70  82.00 120.00  240
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0076325000
_diffrn_orient_matrix_UB_12      0.0068299000
_diffrn_orient_matrix_UB_13      0.0327362000
_diffrn_orient_matrix_UB_21      0.0228567000
_diffrn_orient_matrix_UB_22      -0.0267059000
_diffrn_orient_matrix_UB_23      0.0094352000
_diffrn_orient_matrix_UB_31      0.0275722000
_diffrn_orient_matrix_UB_32      0.0240247000
_diffrn_orient_matrix_UB_33      0.0012122000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            248315
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.099
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_description       block
_exptl_crystal_F_000             4452
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.720
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 7173 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.025(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1038
_refine_ls_number_reflns         17921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+15.7422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0540
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                16525
_reflns_number_total             17921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00644a2.cif
_cod_data_source_block           exp_15712
_cod_depositor_comments
'Adding full bibliography for 7718376--7718378.cif.'
_cod_database_code               7718378
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Ir F '
_shelx_estimated_absorpt_t_max   0.546
_shelx_estimated_absorpt_t_min   0.339
_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:
 C46(H46), C48(H48), C50(H50), C54(H54), C56(H56), C58(H58), C62(H62),
 C64(H64), C66(H66), C70(H70), C72(H72), C74(H74)
2.b Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C13(H13a,H13b,
 H13c), C14(H14a,H14b,H14c), C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C22(H22a,
 H22b,H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C30(H30a,H30b,H30c),
 C31(H31a,H31b,H31c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C34(H34a,H34b,
 H34c), C40(H40a,H40b,H40c), C41(H41a,H41b,H41c), C42(H42a,H42b,H42c), C43(H43a,
 H43b,H43c), C44(H44a,H44b,H44c)
;
_shelx_res_checksum              99098
_shelx_hkl_checksum              76772
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.197
_oxdiff_exptl_absorpt_empirical_full_min 0.651