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_7712893
_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 ad
_chemical_formula_moiety         'C25 H26 Cd Cl2 N2 O, H2 O'
_chemical_formula_sum            'C25 H28 Cd Cl2 N2 O2'
_chemical_formula_weight         571.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-25 deposited with the CCDC.	2023-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.520(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9333(3)
_cell_length_b                   28.6315(14)
_cell_length_c                   12.6065(7)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.80
_cell_measurement_theta_min      2.17
_cell_volume                     2468.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40701
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.032
_diffrn_reflns_theta_min         1.786
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1355 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.8493.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 3735 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         12477
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.735
_reflns_Friedel_fraction_full    0.928
_reflns_Friedel_fraction_max     0.745
_reflns_number_gt                10189
_reflns_number_total             12477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00904a2.cif
_cod_data_source_block           t742
_cod_database_code               7712893
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.840
_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, All O(H,H) groups
2.a Free rotating group:
 O3(H3A,H3B), O4(H4C,H4D)
2.b Ternary CH refined with riding coordinates:
 C17(H17), C1(H1), C19(H19), C5(H5), C17A(H17A), C19A(H19A), C1A(H1A), C5A(H5A)
2.c Secondary CH2 refined with riding coordinates:
 C20A(H20A,H20B), C20(H20C,H20D), C4(H4A,H4B), C23(H23A,H23B), C6(H6A,H6B),
 C23A(H23C,H23D), C7A(H7AA,H7AB), C4A(H4AA,H4AB)
2.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C15A(H15A), C10(H10), C10A(H10A)
2.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C8(H8A,H8B,H8C), C25(H25A,H25B,H25C), C9(H9A,H9B,H9C),
 C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,
 H9AC)
;
_shelx_res_checksum              15669
_olex2_submission_special_instructions 'No special instructions were received'