Preparation and applications of metal complexes supported by fluorene- and anthrone-functionalized (bis)mesoionic 1,2,3-triazol-5-ylidenes
Campos-Dominguez, Emmanuel; Ruiz-Mendoza, Francisco J.; Rendón-Nava, David; Flores-Jarillo, Mariana; Álvarez-Hernández, Alejandro; Mendoza-Espinosa, Daniel; New Journal of Chemistry 49 (2025) 19963–19972; doi:10.1039/D5NJ03832D

data_7064091
_publ_section_title
;
 Preparation and applications of metal complexes supported by fluorene-
 and anthrone-functionalized (bis)mesoionic 1,2,3-triazol-5-ylidenes
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19963
_journal_page_last               19972
_journal_paper_doi               10.1039/D5NJ03832D
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         '2(I), C39 H42 N6, 2.5[C2H3N]'
_chemical_formula_sum            'C44 H49.5 I2 N8.5'
_chemical_formula_weight         951.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-10-22
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-10-23 deposited with the CCDC.	2025-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                110.939(7)
_cell_angle_beta                 105.077(5)
_cell_angle_gamma                96.116(5)
_cell_formula_units_Z            2
_cell_length_a                   11.9940(7)
_cell_length_b                   12.5245(10)
_cell_length_c                   17.3840(11)
_cell_measurement_reflns_used    5375
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.3210
_cell_measurement_theta_min      3.5450
_cell_volume                     2296.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3659
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.768
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -63.00   36.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5235  -37.0000    0.0000 99

  2 omega  -17.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5235   77.0000  150.0000 101

  3 omega  -25.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.0391  -99.0000    0.0000 56

  4 omega  -34.00   64.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.0391   37.0000  -60.0000 98

  5 omega  -25.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.0391  -99.0000 -180.0000 56

  6 omega  -63.00   36.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5235  -37.0000   60.0000 99

  7 omega  -17.00   33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5235   57.0000    0.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0308564000
_diffrn_orient_matrix_UB_12      -0.0594612000
_diffrn_orient_matrix_UB_13      -0.0231534000
_diffrn_orient_matrix_UB_21      -0.0374986000
_diffrn_orient_matrix_UB_22      0.0150321000
_diffrn_orient_matrix_UB_23      -0.0316103000
_diffrn_orient_matrix_UB_31      0.0398228000
_diffrn_orient_matrix_UB_32      -0.0102249000
_diffrn_orient_matrix_UB_33      -0.0243451000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1189
_diffrn_reflns_av_unetI/netI     0.1112
_diffrn_reflns_Laue_measured_fraction_full 0.768
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21403
_diffrn_reflns_point_group_measured_fraction_full 0.768
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.000
_diffrn_reflns_theta_min         3.274
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       Block
_exptl_crystal_F_000             958
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         6367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0681P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3823
_reflns_number_total             6367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03832d2.cif
_cod_data_source_block           dme-195
_cod_depositor_comments
'Adding full bibliography for 7064090--7064094.cif.'
_cod_original_formula_sum        'C44 H49.50 I2 N8.50'
_cod_database_code               7064091
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C12 N3 H26 I2'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C6(H6), C16(H16), C10(H10), C20(H20), C22(H22), C29(H29), C12(H12),
 C9(H9), C8(H8), C7(H7), C11(H11), C36(H36), C34(H34)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C17(H17A,H17B,
 H17C), C26(H26A,H26B,H26C), C38(H38A,H38B,H38C), C33(H33A,H33B,H33C), C39(H39A,
 H39B,H39C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 118 electrons were found in a volume of 
579 A3 in 1 void per unit cell. This is consistent with the presence of 
2.5[C2H3N] per formula unit which account for 110 electrons per unit cell
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'