Crystal structure of poly[(μ2-2-carboxy-5-nitroisophthalato-κ2 O:O′)-(μ2-4-((1H-imidazol-1-yl)methyl)pyridine-κ2 N:N′)zinc(II)], C18H12N4O8Zn
Hong, Dong-Feng; Guo, Wen-Bo; Yin, Wei-Dong; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 1035–1036; doi:10.1515/ncrs-2018-0156

data_8106390
_publ_section_title
;
 Crystal structure of poly[(\m2-2-carboxy-5-nitroisophthalato-\k2
 O:O&#x2032;)-(\m2-4-((1H-imidazol-1-yl)methyl)pyridine-\k2
 N:N&#x2032;)zinc(II)], C18H12N4O8Zn
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1035
_journal_page_last               1036
_journal_paper_doi               10.1515/ncrs-2018-0156
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C18 H12 N4 O8 Zn'
_chemical_formula_sum            'C18 H12 N4 O8 Zn'
_chemical_formula_weight         477.69
_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                 110.525(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5472(6)
_cell_length_b                   21.1662(10)
_cell_length_c                   9.6909(6)
_cell_measurement_reflns_used    4665
_cell_measurement_temperature    291.2(3)
_cell_measurement_theta_max      27.2190
_cell_measurement_theta_min      3.7040
_cell_volume                     1834.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.2(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     35.00  86.00   1.00    7.00    --   13.55 178.00 -90.00   51
  2  \w    -56.00  32.00   1.00    7.00    --   13.55 -38.00  90.00   88
  3  \w    -54.00  30.00   1.00    7.00    --   13.55 -57.00   0.00   84
  4  \w    -80.00 -32.00   1.00    7.00    --  -12.53 -77.00  60.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0105041000
_diffrn_orient_matrix_UB_12      0.0165291000
_diffrn_orient_matrix_UB_13      0.0664374000
_diffrn_orient_matrix_UB_21      0.0488158000
_diffrn_orient_matrix_UB_22      -0.0241654000
_diffrn_orient_matrix_UB_23      0.0402331000
_diffrn_orient_matrix_UB_31      0.0616754000
_diffrn_orient_matrix_UB_32      0.0163192000
_diffrn_orient_matrix_UB_33      -0.0080247000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9731
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.658
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.399
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0258P)^2^+1.9006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2868
_reflns_number_total             3218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0156_suppl.cif
_cod_data_source_block           4033
_cod_database_code               8106390
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C5(H5), C15(H15), C17(H17), C16(H16), C11(H11), C12(H12),
 C18(H18)
2.c Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              41285
_shelx_hkl_checksum              17016
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2017-05-11
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.312
_oxdiff_exptl_absorpt_empirical_full_min 0.699