Circularly polarized blue fluorescence based on chiral heteroleptic six-coordinate <i>bis</i>-pyrazolonate-Zn<sup>2+</sup> complexes.
Liu, Jiaxiang; Zhao, Yuzhen; Zhang, Zhe; Li, Manni; Song, Wenqi; Li, Wentao; Miao, Zongcheng; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6625–6630; doi:10.1039/d4dt00086b

data_7715480
_publ_section_title
;
 Circularly polarized blue fluorescence based on chiral heteroleptic
 six-coordinate <i>bis</i>-pyrazolonate-Zn<sup>2+</sup> complexes.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6625
_journal_page_last               6630
_journal_paper_doi               10.1039/d4dt00086b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C40 H40 N6 O4 Zn, C H4 O'
_chemical_formula_sum            'C41 H44 N6 O5 Zn'
_chemical_formula_weight         766.19
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-10-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-10-09 deposited with the CCDC.	2024-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                67.905(2)
_cell_angle_beta                 83.474(2)
_cell_angle_gamma                70.309(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4625(6)
_cell_length_b                   13.1925(7)
_cell_length_c                   14.4678(7)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      55.146
_cell_measurement_theta_min      3.563
_cell_volume                     1908.38(17)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      200.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49066
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.197
_diffrn_reflns_theta_min         3.563
_diffrn_source_current           2.85
_diffrn_source_power             0.199101
_diffrn_source_voltage           69.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1277 before and 0.0794 after correction.
The Ratio of minimum to maximum transmission is 0.8130.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'yellowish yellow'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       needle
_exptl_crystal_F_000             804
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         14292
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0498P)^2^+0.1417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                12053
_reflns_number_total             14292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00086b2.cif
_cod_data_source_block           20220331fl_0m
_cod_depositor_comments          'Adding full bibliography for 7715480.cif.'
_cod_database_code               7715480
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.840
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.95(3)
 0.05(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3.a Ternary CH refined with riding coordinates:
 C3(H3), C4(H4), C44(H44), C45(H45)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), N2(H2A,H2B), C2(H2C,H2D), C5(H5A,H5B), C6(H6A,H6B),
 N7(H7A,H7B), N8(H8B,H8A), C42(H42A,H42B), C43(H43A,H43B), C46(H46A,H46B),
 C47(H47A,H47B)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C36(H36),
  C37(H37), C38(H38), C39(H39), C40(H40), C48(H48), C49(H49), C50(H50),
 C51(H51), C52(H52), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65),
  C66(H66), C67(H67), C68(H68), C69(H69), C77(H77), C78(H78), C79(H79),
 C80(H80), C81(H81)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C33(H33A,H33B,H33C), C57(H57A,H57B,H57C), C74(H74A,H74B,
 H74C), C41(H41A,H41B,H41C), C82(H82A,H82B,H82C)
3.e Idealised tetrahedral OH refined as rotating group:
 O5(H5), O10(H10A)
;
_olex2_submission_special_instructions 'No special instructions were received'