Synthesis, crystal structures and luminescence properties of Zn(ii) and Cd(ii) coordination compounds assembled from flexible bis(quinolyl) ligands with symmetrical spacers: the influence of coordinated anions
Zhang, Guoqiang; Pan, Rongkai; Liu, Shenggui; Chen, Huihui; CrystEngComm 26 (2024) 6627–6639; doi:10.1039/D4CE00768A

data_7249527
_publ_section_title
;
 Synthesis, crystal structures and luminescence properties of Zn(ii) and
 Cd(ii) coordination compounds assembled from flexible bis(quinolyl)
 ligands with symmetrical spacers: the influence of coordinated anions
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              6627
_journal_page_last               6639
_journal_paper_doi               10.1039/D4CE00768A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C42 H30 Cl4 N12 S2 Zn3, 3(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum            'C51 H55 Cl4 N15 O5 S2 Zn3'
_chemical_formula_weight         1360.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2jct0r
_audit_creation_date             2024-05-09
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-21 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.6452(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6636(5)
_cell_length_b                   23.7116(11)
_cell_length_c                   18.9480(9)
_cell_measurement_reflns_used    4140
_cell_measurement_temperature    302.00(10)
_cell_measurement_theta_max      21.759
_cell_measurement_theta_min      2.188
_cell_volume                     6033.2(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      302.00(10)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture 296K'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1468
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            74449
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.903
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1192 before and 0.0810 after correction.
The Ratio of minimum to maximum transmission is 0.8985.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         10614
_refine_ls_number_restraints     227
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0328P)^2^+8.0464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6465
_reflns_number_total             10614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00768a2.cif
_cod_data_source_block           2335044
_cod_depositor_comments
'Adding full bibliography for 7249521--7249527.cif.'
_cod_database_code               7249527
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.808
_olex2_refinement_description
;
1. Restrained planarity
 C46A, N14A, C48A, C47A
 with sigma of 0.1
2. Uiso/Uaniso restraints and constraints
N13 \\sim C43 \\sim C44 \\sim C45 \\sim O1 \\sim C43A \\sim C44A \\sim C45A
\\sim O1A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C46 \\sim C47 \\sim C48 \\sim N14 \\sim O2 \\sim C46A \\sim C47A \\sim C48A
\\sim N14A \\sim O2A: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
3. Same fragment restrains
{C46A, C47A, C48A, N14A, O2A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C46, C47, C48, N14, O2}
{N13, C43A, C44A, C45A, O1A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{N13, C43, C44, C45, O1}
4. Others
 Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C44A)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=Sof(C45A)=Sof(H45A)=Sof(O1A)=1-FVAR(1)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=
 Sof(C45)=Sof(H45)=Sof(O1)=FVAR(1)
 Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47A)=Sof(H47D)=Sof(H47E)=
 Sof(H47F)=Sof(C48A)=Sof(H48A)=Sof(N14A)=Sof(O2A)=1-FVAR(2)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 Sof(C48)=Sof(H48)=Sof(N14)=Sof(O2)=FVAR(2)
5.a Riding coordinates:
 O4(H4A,H4B)
5.b Free rotating group:
 O5(H5A,H5B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C31(H31), C33(H33), C35(H35), C36(H36),
 C38(H38), C39(H39), C40(H40), C41(H41), N4(H4), N10(H10A), C51(H51), C45(H45),
 C48(H48), C48A(H48A), C45A(H45A)
5.d Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C46A(H46D,H46E,H46F),
 C47A(H47D,H47E,H47F), C43A(H43D,H43E,H43F), C44A(H44D,H44E,H44F)
;
_shelx_res_checksum              76552
_olex2_submission_special_instructions 'No special instructions were received'