Crystal structure of poly[(μ7-4-(3,5-dicarboxylatophenoxy)phthalato)-(1,10-phenanthroline-κ2N,N′)dizinc(II)], C28H14N2O9Zn2
Sun, Tao; Li, Ke; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 1293–1294; doi:10.1515/ncrs-2019-0416

data_8106011
_publ_section_title
;
 Crystal structure of
 poly[(\m7-4-(3,5-dicarboxylatophenoxy)phthalato)-(1,10-phenanthroline-\k2N,N&#x2032;)dizinc(II)],
 C28H14N2O9Zn2
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1293
_journal_page_last               1294
_journal_paper_doi               10.1515/ncrs-2019-0416
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C28 H14 N2 O9 Zn2'
_chemical_formula_sum            'C28 H14 N2 O9 Zn2'
_chemical_formula_weight         653.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                95.202(6)
_cell_angle_beta                 107.027(5)
_cell_angle_gamma                91.896(5)
_cell_formula_units_Z            2
_cell_length_a                   9.6870(5)
_cell_length_b                   10.1849(9)
_cell_length_c                   12.7338(9)
_cell_measurement_reflns_used    6590
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5790
_cell_measurement_theta_min      3.8550
_cell_volume                     1193.97(15)
_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  'XL (Sheldrick, 2008)'
_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 0.998
_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    -33.00  55.00   1.00    1.00    --  -13.80  38.00 -30.00   88
  2  \w    -83.00   5.00   1.00    1.00    --  -13.80 -38.00 150.00   88
  3  \w    -31.00  53.00   1.00    1.00    --  -13.80  57.00-120.00   84
  4  \w     -2.00  82.00   1.00    1.00    --   14.82  57.00  30.00   84
  5  \w    -20.00  54.00   1.00    1.00    --   14.82 -99.00  30.00   74
  6  \w    -20.00  54.00   1.00    1.00    --   14.82 -99.00-150.00   74
  7  \w    -12.00  59.00   1.00    1.00    --   14.82-108.00 -48.00   71
  8  \w    -52.00  32.00   1.00    1.00    --   14.82 -57.00  90.00   84
  9  \w    -12.00  82.00   1.00    1.00    --   14.82  77.00 -90.00   94
 10  \w    -12.00  82.00   1.00    1.00    --   14.82  77.00 120.00   94
 11  \w    -63.00   5.00   1.00    1.00    --  -13.80 117.00  29.92   68
 12  \w    -86.00 -39.00   1.00    1.00    --  -13.80-178.00  30.00   47
 13  \w    -52.00  32.00   1.00    1.00    --   14.82 -57.00 120.00   84
 14  \w    -20.00  46.00   1.00    1.00    --   14.82 -99.00 150.00   66
;
_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      -0.0387934000
_diffrn_orient_matrix_UB_12      -0.0063337000
_diffrn_orient_matrix_UB_13      -0.0570473000
_diffrn_orient_matrix_UB_21      -0.0049610000
_diffrn_orient_matrix_UB_22      -0.0696740000
_diffrn_orient_matrix_UB_23      -0.0002633000
_diffrn_orient_matrix_UB_31      -0.0660134000
_diffrn_orient_matrix_UB_32      0.0038586000
_diffrn_orient_matrix_UB_33      0.0133081000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25935
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.37
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36211
_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_density_diffrn    1.817
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+1.1624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                3738
_reflns_number_total             4433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2019-0416_suppl.cif
_cod_data_source_block           190
_cod_original_cell_volume        1193.97(14)
_cod_database_code               8106011
_chemical_oxdiff_formula         'C H N O Zn'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C15(H15), C17(H17), C19(H19), C21(H21), C22(H22), C25(H25)
;
_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 2.402
_oxdiff_exptl_absorpt_empirical_full_min 0.517