The crystal structure of catena-poly[bis(1-ethylimidazole-k1 N)-(μ 2-benzene-1-carboxyl-3,5-dicarboxylato-κ 2 O, O′)zinc(II)], C19H20N4O6Zn
Guo, Ya-Fei; Chen, Bao-Kuan; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 649–651; doi:10.1515/ncrs-2023-0132

data_8107520
_publ_section_title
;
 The crystal structure of catena-poly[bis(1-ethylimidazole-k1 N)-(\m
 2-benzene-1-carboxyl-3,5-dicarboxylato-\k 2 O, O&#x2032;)zinc(II)],
 C19H20N4O6Zn
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              649
_journal_page_last               651
_journal_paper_doi               10.1515/ncrs-2023-0132
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C19 H20 N4 O6 Zn'
_chemical_formula_sum            'C19 H20 N4 O6 Zn'
_chemical_formula_weight         465.76
_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
_cell_angle_alpha                90
_cell_angle_beta                 97.564(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7411(7)
_cell_length_b                   13.7831(9)
_cell_length_c                   13.5425(10)
_cell_measurement_reflns_used    8232
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.29
_cell_volume                     2172.5(3)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016) [1]'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016) [1]'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016) [1]'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009) [2]'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009) [2]'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015) [3]'
_computing_structure_solution    'XT (Sheldrick, 2015a) [4]'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18959
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.089
_diffrn_reflns_theta_max         25.089
_diffrn_reflns_theta_min         2.118
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.172
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         3838
_refine_ls_number_restraints     658
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0645
_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^)+(0.0635P)^2^+6.4181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1643
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2571
_reflns_number_total             3838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0132_suppl_001.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8107520
_shelx_estimated_absorpt_t_max   0.799
_shelx_estimated_absorpt_t_min   0.766
_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 C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C5-C19 = N3-C5
 1.5 with sigma of 0.01
 N3-C15
 1.5 with sigma of 0.01
 C7-C2
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim N1 \\sim N2
\\sim N3 \\sim N4: within 3.8A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 3.8A
Uanis(C15) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.01
Uanis(C11) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C19) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C5(0.8) H5A(0.8) H5B(0.8) C9(0.35) H9A(0.35) H9B(0.35) H9C(0.35)
 C11(0.6) H11(0.6) C13(0.4) H13(0.4) C15(0.2) H15A(0.2) H15B(0.2) C17(0.4)
 H17(0.4) C19(0.65) H19A(0.65) H19B(0.65) H19C(0.65) C21(0.6) H21(0.6)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C15(H15A,H15B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C10(H10), C11(H11), C13(H13), C17(H17), C18(H18), C20(H20),
 C21(H21), C22(H22), C23(H23)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C)
5.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              10691
_shelx_hkl_checksum              58262
_olex2_submission_special_instructions 'No special instructions were received'