Efficient emission of Zn(II) and Cd(II) complexes with nopinane-annelated 4,5-diazafluorene and 4,5-diazafluoren-9-one ligands: how slight structural modification alters fluorescence mechanism
Kokina, T. E.; Shekhovtsov, Nikita; Vasilyev, Evgene S.; Glinskaya, Ludmila; Mikheilis, Alexsandr V.; Plyusnin, Victor F.; Tkachev, Alexey V.; Bushuev, Mark B.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00904A

data_7712892
_publ_section_title
;
 Efficient emission of Zn(II) and Cd(II) complexes with nopinane-annelated
 4,5-diazafluorene and 4,5-diazafluoren-9-one ligands: how slight
 structural modification alters fluorescence mechanism
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00904A
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C25 H26 Cl2 N2 O Zn, C2 H2 N'
_chemical_formula_sum            'C27 H28 Cl2 N3 O Zn'
_chemical_formula_weight         546.79
_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             2022-02-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-09 deposited with the CCDC.	2023-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2980(5)
_cell_length_b                   14.6532(7)
_cell_length_c                   17.2961(9)
_cell_measurement_reflns_used    9285
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      2.30
_cell_volume                     2610.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Bruker Apex DUO CCD area-detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39080
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.095
_diffrn_reflns_theta_min         1.821
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 2097 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         7626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0419
_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/[\s^2^(Fo^2^)+(0.0482P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0941
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.889
_reflns_number_gt                5839
_reflns_number_total             7626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00904a2.cif
_cod_data_source_block           t685
_cod_database_code               7712892
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.800
_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. Others
 Fixed Sof: H16a(0.5) H16b(0.5)
3.a Ternary CH refined with riding coordinates:
 C1(H1), C1A(H1A), C5(H5), C5A(H5A)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b), C4A(H4Aa,H4Ab), C7(H7a,H7b), C7A(H7Aa,H7Ab)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C10A(H10A)
3.d Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C8A(H8Aa,H8Ab,H8Ac), C9(H9a,H9b,H9c), C9A(H9Aa,H9Ab,H9Ac),
 C16(H16a,H16b,H16c)
;
_shelx_res_checksum              15223
_olex2_submission_special_instructions 'No special instructions were received'