Crystal structure of the coordination polymer catena-poly[(1,2-di(pyridin-4-yl)ethane-κN)-(μ2-2-nitroisophthalato-κ2O:O′)zinc(II)], C20H17N3O7Zn
Liu, Guang-Zhen; Ma, Lu-Ping; Jia, Ru; Zeitschrift für Kristallographie - New Crystal Structures 235 (2019) 87–89; doi:10.1515/ncrs-2019-0510

data_8105026
_publ_section_title
;
 Crystal structure of the coordination polymer
 catena-poly[(1,2-di(pyridin-4-yl)ethane-\kN)-(\m2-2-nitroisophthalato-\k2O:O&#x2032;)zinc(II)],
 C20H17N3O7Zn
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              87
_journal_page_last               89
_journal_paper_doi               10.1515/ncrs-2019-0510
_journal_volume                  235
_journal_year                    2019
_chemical_formula_moiety         'C20 H17 N3 O7 Zn'
_chemical_formula_sum            'C20 H17 N3 O7 Zn'
_chemical_formula_weight         476.73
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 101.900(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4368(3)
_cell_length_b                   15.1527(5)
_cell_length_c                   12.9007(3)
_cell_measurement_reflns_used    7445
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5600
_cell_measurement_theta_min      3.8780
_cell_volume                     1996.34(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.887
_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    -20.00  25.00   1.00   10.00    --  -13.80 -99.00  30.00   45
  2  \w    -20.00  25.00   1.00   10.00    --  -13.80 -99.00-120.00   45
  3  \w    -31.00  53.00   1.00   10.00    --  -13.80  57.00   0.00   84
  4  \w    -54.00  34.00   1.00   10.00    --   14.82 -38.00   0.00   88
  5  \w    -53.00  42.00   1.00   10.00    --   14.82 -77.00 120.00   95
  6  \w    -12.00  82.00   1.00   10.00    --   14.82  77.00-120.00   94
  7  \w    -81.00 -56.00   1.00   10.00    --  -13.80 -57.00   0.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0538439000
_diffrn_orient_matrix_UB_12      0.0293244000
_diffrn_orient_matrix_UB_13      0.0133383000
_diffrn_orient_matrix_UB_21      -0.0418285000
_diffrn_orient_matrix_UB_22      0.0325347000
_diffrn_orient_matrix_UB_23      0.0146134000
_diffrn_orient_matrix_UB_31      0.0132659000
_diffrn_orient_matrix_UB_32      -0.0164708000
_diffrn_orient_matrix_UB_33      0.0526037000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20317
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.462
_diffrn_reflns_theta_min         3.348
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.586
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0322P)^2^+1.5584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3729
_reflns_number_total             4466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0510_suppl.cif
_cod_data_source_block           lgz-36
_cod_original_cell_volume        1996.36(10)
_cod_database_code               8105026
_chemical_oxdiff_usercomment     Y202-Co
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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.a Rotating group:
 O1W(H1WA,H1WB)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C12(H12), C13(H13), C17(H17),
 C18(H18), C19(H19), C20(H20)
;