Design and synthesis of diverse Cd<sup>2+</sup>/Zn<sup>2+</sup>/Cu<sup>2+</sup> coordination polymers tuned by dicarboxylate and auxiliary 1,4-bis(pyridin-4-ylmethyl)piperazine ligands with luminescence and Hirshfeld surface analyses.
Jin, Nanhao; Liu, Yuqi; Dai, Siyu; Li, Yanghua; Wang, Xinying; Zhao, Yue; Liu, Xiaoming; Chen, Han; Luo, Huilong; Li, Wei; Acta crystallographica Section B, Structural science, crystal engineering and materials 79 (2023) –; doi:10.1107/S2052520623007813

data_2312357
_publ_section_title
;
 Design and synthesis of diverse
 Cd<sup>2+</sup>/Zn<sup>2+</sup>/Cu<sup>2+</sup> coordination polymers
 tuned by dicarboxylate and auxiliary
 1,4-bis(pyridin-4-ylmethyl)piperazine ligands with luminescence and
 Hirshfeld surface analyses.
;
_journal_coeditor_code           AW5080
_journal_issue                   6
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_paper_doi               10.1107/S2052520623007813
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          '[Cu (C4 H2 O4) (C16 H20 N4) (H2 O)2]'
_chemical_formula_moiety         'C20 H22 Cu N4 O4, 2(H2 O)'
_chemical_formula_sum            'C20 H26 Cu N4 O6'
_chemical_formula_weight         481.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-30
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.302(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.829(3)
_cell_length_b                   12.668(4)
_cell_length_c                   10.008(3)
_cell_measurement_reflns_used    1687
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.471
_cell_measurement_theta_min      2.828
_cell_volume                     1110.3(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3393
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.675
_diffrn_reflns_theta_min         2.828
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0469 before and 0.0370 after correction.
The Ratio of minimum to maximum transmission is 0.8576.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       block
_exptl_crystal_F_000             502
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         1304
_refine_ls_number_restraints     347
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+0.2284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1168
_reflns_number_total             1304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            aw5080sup1.cif
_cod_data_source_block           4
_cod_database_code               2312357
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.895
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N2-C8 = N2-C9 = N2-C11 = N3-C10 = N3-C12 = N3-C13
 1.47 with sigma of 0.01
 C14-C13 = C5-C8
 1.5 with sigma of 0.01
 C9-C10 = C12-C11
 1.54 with sigma of 0.01
 C11-C8 = C12-C13
 2.401 with sigma of 0.02
 C11-C9 = C12-C10
 2.401 with sigma of 0.02
 C8-C9 = C10-C13
 2.401 with sigma of 0.02
 C11-N3 = C10-N2
 2.458 with sigma of 0.02
 C9-N3 = N2-C12
 2.458 with sigma of 0.02
 C15-C13 \\sim C18-C13
 with sigma of 0.02
3. Restrained planarity
 N1, C3, C4, C5, C6, C7, C8
 with sigma of 0.1
 N4, C13, C14, C15, C16, C17, C18
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N1 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim N3 \\sim N4 \\sim C16
\\sim C15 \\sim C14 \\sim C18 \\sim C17 \\sim C9 \\sim C10 \\sim C11 \\sim C12
\\sim C13 \\sim N2 \\sim C8: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(C10) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C7) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
5. Rigid body (RIGU) restrains
 N1, N3, N4, C3, C4, C5, C6, C7, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, N2, C8, Cu1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Fixed Sof: N1(0.25) C3(0.25) H3(0.25) C4(0.25) H4(0.25) C5(0.25) C6(0.25)
 H6(0.25) C7(0.25) H7(0.25) N3(0.25) N4(0.25) C16(0.25) H16(0.25) C15(0.25)
 H15(0.25) C14(0.25) C18(0.25) H18(0.25) C17(0.25) H17(0.25) C9(0.25) H9A(0.25)
 H9B(0.25) C10(0.25) H10A(0.25) H10B(0.25) C11(0.25) H11A(0.25) H11B(0.25)
 C12(0.25) H12A(0.25) H12B(0.25) C13(0.25) H13A(0.25) H13B(0.25) N2(0.25)
 C8(0.25) H8A(0.25) H8B(0.25) O1W(0.5) H1WA(0.5) H1WB(0.5) O2(0.5) C1(0.5)
 C2(0.5) H2(0.5)
7.a Riding coordinates:
 O1W(H1WA,H1WB)
7.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C8(H8A,H8B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C16(H16), C15(H15), C18(H18), C17(H17)
7.d Fitted hexagon refined as free rotating group:
 N1(C3,C4,C5,C6,C7), N4(C16,C15,C14,C18,C17)
;
_shelx_res_checksum              58374
_shelx_hkl_checksum              17908
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2312357