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_7064093
_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         'C37 H36 N6'
_chemical_formula_sum            'C37 H36 N6'
_chemical_formula_weight         564.72
_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     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                90
_cell_angle_beta                 101.275(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6174(13)
_cell_length_b                   8.1610(6)
_cell_length_c                   24.7494(19)
_cell_measurement_reflns_used    9165
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.7640
_cell_measurement_theta_min      3.3790
_cell_volume                     3093.5(4)
_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
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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 0.971
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -34.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610   37.0000 -150.0000 99

  2 omega  -82.00   19.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  -77.0000   60.0000 101

  3 omega  -38.00   63.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610   57.0000  120.0000 101

  4 omega  -25.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  -99.0000  -90.0000 56

  5 omega  -25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000  -30.0000 77

  6 omega  -17.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454   57.0000 -120.0000 102

  7 omega  -13.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454   37.0000  150.0000 99

  8 omega  -25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000   90.0000 77

  9 omega  -25.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  -99.0000 -180.0000 56

 10 omega  -51.00    4.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610   99.0000 -159.0000 55

 11 omega  -25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000 -150.0000 77

 12 omega  -25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000   30.0000 77

 13 omega  -25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000  -90.0000 77

 14 omega  -13.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454   37.0000    0.0000 99

 15 omega  -25.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  -99.0000    0.0000 56

 16 omega  -25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000  -60.0000 77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0097302000
_diffrn_orient_matrix_UB_12      0.0528420000
_diffrn_orient_matrix_UB_13      -0.0231383000
_diffrn_orient_matrix_UB_21      0.0246404000
_diffrn_orient_matrix_UB_22      0.0633073000
_diffrn_orient_matrix_UB_23      0.0154285000
_diffrn_orient_matrix_UB_31      0.0379913000
_diffrn_orient_matrix_UB_32      -0.0274501000
_diffrn_orient_matrix_UB_33      -0.0089588000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            46453
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.023
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76248
_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    1.213
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.0014(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0665P)^2^+1.5944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2029
_reflns_number_total             2726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03832d2.cif
_cod_data_source_block           dme-193
_cod_depositor_comments
'Adding full bibliography for 7064090--7064094.cif.'
_cod_database_code               7064093
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C12 H26 N6'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C19(H19), C5(H5), C16(H16), C18(H18), C17(H17)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_olex2_submission_special_instructions 'No special instructions were received'