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_7718376
_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 H61 Ir4 N8, C44 H60 Ir4 N8, 2(C4 H10 O)'
_chemical_formula_sum            'C96 H141 Ir8 N16 O2'
_chemical_formula_weight         3088.84
_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   mixed
_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                 101.540(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.1212(7)
_cell_length_b                   17.7347(3)
_cell_length_c                   16.6640(3)
_cell_measurement_reflns_used    29852
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      29.4110
_cell_measurement_theta_min      2.1590
_cell_volume                     9880.0(3)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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   -105.00  17.00   0.50    2.11    --  -15.70 -57.00-150.00  244
  2  \w    -57.00   3.00   0.50    2.11    --   15.80  19.00-150.00  120
  3  \w     22.00  56.00   0.50    2.11    --   15.80  19.00-150.00   68
  4  \w    -49.00 100.00   0.50    2.11    --   15.80  19.00   0.00  298
;
_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      -0.0157448000
_diffrn_orient_matrix_UB_12      -0.0124246000
_diffrn_orient_matrix_UB_13      0.0187993000
_diffrn_orient_matrix_UB_21      -0.0018080000
_diffrn_orient_matrix_UB_22      -0.0333572000
_diffrn_orient_matrix_UB_23      -0.0239373000
_diffrn_orient_matrix_UB_31      0.0141059000
_diffrn_orient_matrix_UB_32      -0.0182539000
_diffrn_orient_matrix_UB_33      0.0309870000
_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  0.0260
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            74256
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.229
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.784
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27851
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_description       block
_exptl_crystal_F_000             5844
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.179
_refine_diff_density_min         -2.323
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1146
_refine_ls_number_reflns         22574
_refine_ls_number_restraints     738
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0084P)^2^+107.6492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16423
_reflns_number_total             22574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00644a2.cif
_cod_data_source_block           exp_13505
_cod_depositor_comments
'Adding full bibliography for 7718376--7718378.cif.'
_cod_database_code               7718376
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Li C N H O Cl Ir'
_shelx_estimated_absorpt_t_max   0.412
_shelx_estimated_absorpt_t_min   0.222
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C95-C96
 1.54 with sigma of 0.02
 C93-C94
 1.54 with sigma of 0.02
 C95-O2
 1.54 with sigma of 0.01
 C96-C95
 1.54 with sigma of 0.01
 O2-C94
 1.54 with sigma of 0.01
 C94-C93
 1.54 with sigma of 0.01
 C92-O1
 2.5 with sigma of 0.01
 C91-C90
 2.5 with sigma of 0.01
 O1-C89
 2.5 with sigma of 0.01
 C95-C94
 2.5 with sigma of 0.04
 C96-O2
 2.5 with sigma of 0.04
 O2-C93
 2.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim
C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim
C65 \\sim C66 \\sim C67 \\sim C68: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3A
C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13
\\sim C14: within 3A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3A
O1 \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim O2 \\sim C93 \\sim C94 \\sim
C95 \\sim C96: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3A
Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq,
Uanis(C53) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C95)
\\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C90) \\sim Ueq,
Uanis(O1) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C90(H90A,H90B), C91(H91A,H91B), C94(H94A,H94B), C95(H95A,H95B)
4.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), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C),
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C64(H64A,H64B,
 H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,
 H68B,H68C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C),
 C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C84(H84A,H84B,H84C), C85(H85A,H85B,
 H85C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C89(H89A,
 H89B,H89C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C96(H96A,H96B,H96C)
;
_shelx_res_checksum              77583
_shelx_hkl_checksum              27703
_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 2.434
_oxdiff_exptl_absorpt_empirical_full_min 0.803