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_7249526
_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 Cd4 I6 N12 S2, 2(C3 H7 N O)'
_chemical_formula_sum            'C48 H44 Cd4 I6 N14 O2 S2'
_chemical_formula_weight         2124.09
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2jct3v
_audit_creation_date             2024-05-28
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-07-28 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.152(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4958(5)
_cell_length_b                   13.0911(6)
_cell_length_c                   18.1432(10)
_cell_measurement_reflns_used    7058
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      25.4560
_cell_measurement_theta_min      3.9230
_cell_volume                     3094.0(3)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector_area_resol_mean 8.0606
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.891
_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    -24.00  52.00   1.00    5.00    --  -16.28  38.00 -30.00   76
  2  \w     24.00  52.00   1.00    5.00    --   15.49  77.00 -60.00   28
  3  \w     19.00  47.00   1.00    5.00    --   15.49  57.00  30.00   28
  4  \w      0.00  33.00   1.00    5.00    --   15.49  19.00-120.00   33
  5  \w    -25.00  22.00   1.00    5.00    --  -16.28 -99.00  90.00   47
  6  \w    -48.00  42.00   1.00    5.00    --   15.49 -77.00 -90.00   90
  7  \w     41.00  84.00   1.00    5.00    --   15.49-178.00-180.00   43
  8  \w    -80.00  -3.00   1.00    5.00    --  -16.28 -57.00 150.00   77
  9  \w    -83.00   9.00   1.00    5.00    --  -16.28 -77.00  30.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33694
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.490
_diffrn_reflns_theta_min         3.375
_exptl_absorpt_coefficient_mu    4.466
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58866
_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 light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.280
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7663
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+7.0519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5346
_reflns_number_total             7663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00768a2.cif
_cod_data_source_block           2335047
_cod_depositor_comments
'Adding full bibliography for 7249521--7249527.cif.'
_cod_database_code               7249526
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.574
_shelx_estimated_absorpt_t_min   0.535
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 C22, C23A, C24A, N7A
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Cd1 \\sim Cd2 \\sim I2 \\sim I3 \\sim I1 \\sim I1A \\sim IIB: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C22 \\sim O1 \\sim C23 \\sim C24 \\sim N7 \\sim C23A \\sim C24A \\sim N7A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(I1) \\sim Ueq, Uanis(I1A) \\sim Ueq, Uanis(IIB) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{C22, O1, C23A, C24A, N7A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C22, O1, C23, C24, N7}
5. Others
 1*[Sof(I1)]+1*[Sof(I1A)]+1*[Sof(IIB)]=1 with esd of 0
 Sof(H22A)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24D)=
 Sof(H24E)=Sof(H24F)=Sof(N7A)=1-FVAR(1)
 Sof(H22)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=Sof(N7)=FVAR(1)
6.a 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), N4(H4), C22(H22), C22(H22A)
6.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C23A(H23D,H23E,H23F), C24A(H24D,
 H24E,H24F)
;
_shelx_res_checksum              10434
_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
;