Crystal structure of poly[diaqua-(μ 2-1,3-di(1H-imidazol-1-yl)propane-κ 2 N:N′)-bis(μ 2-5-carboxybenzene-1,3-dicarboxylato-O,O′:O″)-aqua-di-zinc dihydrate solvate], C27H28N4O16Zn2
Zhang, Yan; Wang, Jia-Xin; Huang, Pei-Pei; Wu, Ting-Ting; Gao, Jia-Hao; Lu, Jiu-Fu; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 991–993; doi:10.1515/ncrs-2023-0315

data_8107620
_publ_section_title
;
 Crystal structure of poly[diaqua-(\m 2-1,3-di(1H-imidazol-1-yl)propane-\k
 2 N:N&#x2032;)-bis(\m
 2-5-carboxybenzene-1,3-dicarboxylato-O,O&#x2032;:O&#x2033;)-aqua-di-zinc
 dihydrate solvate], C27H28N4O16Zn2
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              991
_journal_page_last               993
_journal_paper_doi               10.1515/ncrs-2023-0315
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C27 H24 N4 O14 Zn2, 2(H2 O)'
_chemical_formula_sum            'C27 H28 N4 O16 Zn2'
_chemical_formula_weight         795.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 95.373(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0720(3)
_cell_length_b                   15.7589(5)
_cell_length_c                   14.9320(6)
_cell_measurement_reflns_used    1779
_cell_measurement_temperature    294.23(10)
_cell_measurement_theta_max      28.2110
_cell_measurement_theta_min      3.7620
_cell_volume                     3062.48(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      294.23(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   35.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  178.0000 -150.0000 42

  2 omega  -25.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   19.0000  -90.0000 123

  3 omega   33.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   77.0000  -60.0000 62
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0085887000
_diffrn_orient_matrix_UB_12      0.0323761000
_diffrn_orient_matrix_UB_13      -0.0328569000
_diffrn_orient_matrix_UB_21      -0.0536698000
_diffrn_orient_matrix_UB_22      -0.0074169000
_diffrn_orient_matrix_UB_23      -0.0018183000
_diffrn_orient_matrix_UB_31      -0.0039643000
_diffrn_orient_matrix_UB_32      0.0303668000
_diffrn_orient_matrix_UB_33      0.0345577000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5808
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.527
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.046
_refine_diff_density_min         -1.547
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3012
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0265P)^2^+14.9053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2478
_reflns_number_total             3012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0315_suppl_001.cif
_cod_data_source_block           1
_cod_original_cell_volume        3062.48(18)
_cod_database_code               8107620
_chemical_oxdiff_formula         'C H N O Zn'
_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
 H4-O4
 0.88 with sigma of 0.01
 H8A-O8
 0.88 with sigma of 0.01
 H8B-O8
 0.88 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Zn1 \\sim O7: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.001 within 2A
Uanis(Zn1) = Uanis(O7)
4. Others
 Fixed Sof: H14A(0.5) H14B(0.5)
5.a Rotating group:
 O7(H7A,H7B)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12)
;
_shelx_res_checksum              70481
_shelx_hkl_checksum              91357
_olex2_date_sample_data_collection 2016-12-05
_olex2_submission_special_instructions 'No special instructions were received'