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_7249523
_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         'C24 H24 Cd2 I3 N7 O3, C3 H7 N O, 0.25(H2 O)'
_chemical_formula_sum            'C27 H31.5 Cd2 I3 N8 O4.25'
_chemical_formula_weight         1141.60
_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     dual
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2jcsyn
_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                60.806(15)
_cell_angle_beta                 67.338(12)
_cell_angle_gamma                81.515(9)
_cell_formula_units_Z            2
_cell_length_a                   12.5273(11)
_cell_length_b                   13.4647(17)
_cell_length_c                   13.625(2)
_cell_measurement_reflns_used    3546
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      23.4330
_cell_measurement_theta_min      4.2030
_cell_volume                     1849.1(5)
_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(2)
_diffrn_detector_area_resol_mean 8.0606
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.821
_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    -16.00  25.00   1.00    5.00    --   15.49 -57.00   0.00   41
  2  \w     -7.00  21.00   1.00    5.00    --  -16.28 -99.00   0.00   28
  3  \w    -25.00   0.00   1.00    5.00    --  -16.28 -99.00-120.00   25
  4  \w     29.00  54.00   1.00    5.00    --   15.49 -99.00-180.00   25
  5  \w    -36.00  47.00   1.00    5.00    --  -16.28  19.00-120.00   83
  6  \w     -9.00  82.00   1.00    5.00    --   15.49  77.00 -60.00   91
  7  \w    -25.00  51.00   1.00    5.00    --   15.49 -99.00 150.00   76
  8  \w    -46.00   2.00   1.00    5.00    --  -16.28  19.00 150.00   48
;
_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  0.0532
_diffrn_reflns_av_unetI/netI     0.1022
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17122
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.656
_diffrn_reflns_theta_min         3.426
_exptl_absorpt_coefficient_mu    3.697
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57126
_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    2.050
_exptl_crystal_description       block
_exptl_crystal_F_000             1077
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.079
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.143
_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     490
_refine_ls_number_reflns         8591
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0381P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4831
_reflns_number_total             8591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00768a2.cif
_cod_data_source_block           2335042
_cod_depositor_comments
'Adding full bibliography for 7249521--7249527.cif.'
_cod_original_cell_volume        1849.0(5)
_cod_original_formula_sum        'C27 H31.50 Cd2 I3 N8 O4.25'
_cod_database_code               7249523
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.626
_shelx_estimated_absorpt_t_min   0.589
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained planarity
 C27, N8, C25A, C26A
 with sigma of 0.1
 C27, N8, C25, C26
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
N8 \\sim C25 \\sim C26 \\sim C25A \\sim C26A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O3 \\sim C22 \\sim C23 \\sim C24 \\sim N7 \\sim C22A \\sim C23A \\sim C24A
\\sim N7A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Cd1 \\sim I1 \\sim I2 \\sim I1A \\sim I2A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{Cd1, I1A, I2A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{Cd1, I1, I2}
{O3, C22A, C23A, C24A, N7A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{O3, C22, C23, C24, N7}
{N8, C25A, C26A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{N8, C25, C26}
5. Others
 Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C24A)=Sof(H24A)=Sof(N7A)=1-FVAR(1)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 Sof(C24)=Sof(H24)=Sof(N7)=FVAR(1)
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=
 Sof(H26F)=1-FVAR(2)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 FVAR(2)
 Sof(I1A)=Sof(I2A)=1-FVAR(3)
 Sof(I1)=Sof(I2)=FVAR(3)
 Fixed Sof: O5(0.25) H5A(0.25) H5B(0.25)
6.a Riding coordinates:
 O5(H5A,H5B)
6.b Rotating group:
 O2(H2A,H2B)
6.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), N4(H4), C24(H24), C27(H27),
 C24A(H24A)
6.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C22A(H22D,H22E,H22F), C23A(H23D,H23E,H23F), C25A(H25D,H25E,H25F),
 C26A(H26D,H26E,H26F)
;
_shelx_res_checksum              61058
_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
;