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_7249522
_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 H32 Cl4 N12 O2 S2 Zn4, 3(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum            'C51 H57 Cl4 N15 O7 S2 Zn4'
_chemical_formula_weight         1459.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-09-01
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-01 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                110.603(11)
_cell_angle_beta                 97.125(10)
_cell_angle_gamma                101.299(11)
_cell_formula_units_Z            1
_cell_length_a                   11.0646(14)
_cell_length_b                   11.8428(15)
_cell_length_c                   12.9025(15)
_cell_measurement_reflns_used    1311
_cell_measurement_temperature    170
_cell_measurement_theta_max      19.5750
_cell_measurement_theta_min      3.8250
_cell_volume                     1517.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0606
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -47.00  32.00   1.00    7.50    --   15.34 -57.00 -30.00   79
  2  \w    -19.00  20.00   1.00    7.50    --  -16.28 -99.00-120.00   39
  3  \w    -45.00  32.00   1.00    7.50    --   15.34 -57.00-150.00   77
  4  \w    -11.00  44.00   1.00    7.50    --   15.34  77.00-150.00   55
  5  \w     29.00  54.00   1.00    7.50    --   15.34 -99.00  90.00   25
  6  \w    -52.00  30.00   1.00    7.50    --   15.34 -57.00  90.00   82
  7  \w     -1.00  35.00   1.00    7.50    --   15.34  57.00  90.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0553548000
_diffrn_orient_matrix_UB_12      0.0196498000
_diffrn_orient_matrix_UB_13      -0.0182388000
_diffrn_orient_matrix_UB_21      -0.0105552000
_diffrn_orient_matrix_UB_22      0.0602633000
_diffrn_orient_matrix_UB_23      0.0137822000
_diffrn_orient_matrix_UB_31      0.0359947000
_diffrn_orient_matrix_UB_32      0.0191872000
_diffrn_orient_matrix_UB_33      0.0555530000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0914
_diffrn_reflns_av_unetI/netI     0.1748
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11409
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.451
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.869
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         5328
_refine_ls_number_restraints     442
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.1652
_refine_ls_R_factor_gt           0.0821
_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^)+(0.0587P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2807
_reflns_number_total             5328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00768a2.cif
_cod_data_source_block           exp_11810
_cod_depositor_comments
'Adding full bibliography for 7249521--7249527.cif.'
_cod_original_cell_volume        1517.2(3)
_cod_database_code               7249522
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.767
_shelx_estimated_absorpt_t_min   0.730
_olex2_refinement_description
;
1. Restrained distances
 C26-O4
 1.22 with sigma of 0.02
 C26-N8
 1.36 with sigma of 0.02
 O3-C23
 2.79 with sigma of 0.02
 N8-C27
 1.45 with sigma of 0.02
 N8-C25
 1.46 with sigma of 0.02
 H2B-H19_$1
 2.1 with sigma of 0.02
 H1-H2A
 2.1 with sigma of 0.02
 C26-C27
 2.46 with sigma of 0.04
 C26-C25
 2.45 with sigma of 0.04
 C26-O4
 2.797 with sigma of 0.02
 N8-C26
 1.2164 with sigma of 0.02
 C25-C26
 2.4456 with sigma of 0.02
 O4-C26
 2.4456 with sigma of 0.02
 O4-N8
 2.2984 with sigma of 0.02
 N8-C27
 1.4503 with sigma of 0.02
 C25-C27
 2.4578 with sigma of 0.02
 O4-C25
 1.2164 with sigma of 0.02
 C25-N8
 1.3625 with sigma of 0.02
 N8-C27 \\sim N8-C25
 with sigma of 0.02
2. Restrained planarity
 C26, O4, N8, C27, C25
 with sigma of 0.1
 C26, O4, N8, C25, C27
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C26 \\sim O4 \\sim N8 \\sim C27 \\sim C25: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C26 \\sim N8 \\sim C27 \\sim C25 \\sim O4: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N8) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C26, O4, N8, C27, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) O4(0.5) N8(0.5) C27(0.5)
 H27A(0.5) H27B(0.5) H27C(0.5) C25(0.5) H25(0.5)
6.a Riding coordinates:
 O1(H1), C26(H26A,H26B,H26C)
6.b Free rotating group:
 O2(H2A,H2B)
6.c Aromatic/amide H refined with riding coordinates:
 N4(H4), C10(H10), C2(H2), C5(H5), C3(H3), C15(H15), C12(H12), C6(H6), C8(H8),
 C20(H20), C18(H18), C19(H19), C17(H17), C7(H7), C14(H14), C22(H22), C25(H25)
6.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              7318
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.272
_oxdiff_exptl_absorpt_empirical_full_min 0.780