Crystal structure of poly[aqua-(μ 2-3,3′,4,5′-biphenyl tetracarboxylate- κ 3 O,O′:O′′) -(μ 2-4,4′-bis(pyrid-4-yl)biphenyl-κ 2 N:N′)zinc(II)], C27H18NO9Zn
Luo, Jie; Wang, Xiao-Wei; Zheng, Ying-Li; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 117–119; doi:10.1515/ncrs-2020-0411

data_8104898
_publ_section_title
;
 Crystal structure of poly[aqua-(\m 2-3,3&#x2032;,4,5&#x2032;-biphenyl
 tetracarboxylate- \k 3 O,O&#x2032;:O&#x2032;&#x2032;) -(\m
 2-4,4&#x2032;-bis(pyrid-4-yl)biphenyl-\k 2 N:N&#x2032;)zinc(II)],
 C27H18NO9Zn
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              117
_journal_page_last               119
_journal_paper_doi               10.1515/ncrs-2020-0411
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C27 H18 N O9 Zn'
_chemical_formula_sum            'C27 H18 N O9 Zn'
_chemical_formula_weight         565.79
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                83.830(7)
_cell_angle_beta                 84.306(8)
_cell_angle_gamma                89.406(9)
_cell_formula_units_Z            2
_cell_length_a                   8.4357(10)
_cell_length_b                   10.1228(10)
_cell_length_c                   13.5186(10)
_cell_measurement_reflns_used    3010
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9480
_cell_measurement_theta_min      3.8360
_cell_volume                     1142.0(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    9.80    --  -13.48 -99.00   0.00   45
  2  \w    -20.00  25.00   1.00    9.80    --  -13.48 -99.00 -60.00   45
  3  \w    -81.00   3.00   1.00    9.80    --  -13.48 -57.00 -30.00   84
  4  \w    -20.00  25.00   1.00    9.80    --  -13.48 -99.00-180.00   45
  5  \w    -86.00 -35.00   1.00    9.80    --  -13.48-178.00-180.00   51
  6  \w     -4.00  84.00   1.00    9.80    --   14.49  38.00-180.00   88
  7  \w    -57.00  44.00   1.00    9.80    --   14.49 -19.00   0.00  101
  8  \w    -30.00  -1.00   1.00    9.80    --  -13.48  57.00 120.00   29
  9  \w     35.00  87.00   1.00    9.80    --   14.49 178.00 -90.00   52
;
_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      0.0516379000
_diffrn_orient_matrix_UB_12      0.0538695000
_diffrn_orient_matrix_UB_13      0.0033044000
_diffrn_orient_matrix_UB_21      0.0322154000
_diffrn_orient_matrix_UB_22      -0.0361112000
_diffrn_orient_matrix_UB_23      0.0413261000
_diffrn_orient_matrix_UB_31      0.0587107000
_diffrn_orient_matrix_UB_32      -0.0275984000
_diffrn_orient_matrix_UB_33      -0.0331113000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0956
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12566
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42190
_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_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             578
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4227
_refine_ls_number_restraints     1050
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.8042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1427
_reflns_number_gt                3150
_reflns_number_total             4227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_j_ncrs-2020-0411_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        1142.05(19)
_cod_database_code               8104898
_chemical_oxdiff_formula         'c h n o zn'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. 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 C24 \\sim C25
\\sim C26 \\sim C27: within 7A with sigma of 0.01 and sigma for terminal atoms
of 0.02
3.a Riding coordinates:
 O1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C6(H6A), C9(H9), C11(H11), C13(H13), C17(H17), C18(H18),
 C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27)
3.c Idealised tetrahedral OH refined as rotating group:
 O4(H4), O6(H6)
;