Hydrothermal synthesis and crystal structure of catena-poly[bis(4-((pyridin-4-ylmethyl)amino)benzoato-κ3 N:O,O′)zinc(II) – 1,2-di(pyridin-4-yl)ethene – water (1/1/1), C38H34N6O5Zn
Wei-Dong, Yin; Yu-Ying, He; Jia, Shen; Gui-Lian, Li; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 211–213; doi:10.1515/ncrs-2018-0217

data_8105593
_publ_section_title
;
 Hydrothermal synthesis and crystal structure of
 catena-poly[bis(4-((pyridin-4-ylmethyl)amino)benzoato-\k3
 N:O,O&#x2032;)zinc(II) -- 1,2-di(pyridin-4-yl)ethene -- water (1/1/1),
 C38H34N6O5Zn
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              211
_journal_page_last               213
_journal_paper_doi               10.1515/ncrs-2018-0217
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C26 H22 N4 O4 Zn, H2 O, C12 H10 N2'
_chemical_formula_sum            'C38 H34 N6 O5 Zn'
_chemical_formula_weight         720.08
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                102.770(4)
_cell_angle_beta                 90.522(3)
_cell_angle_gamma                100.879(4)
_cell_formula_units_Z            2
_cell_length_a                   9.1991(4)
_cell_length_b                   9.7349(4)
_cell_length_c                   19.5840(8)
_cell_measurement_reflns_used    5333
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.7800
_cell_measurement_theta_min      3.9710
_cell_volume                     1677.31(13)
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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     -2.00  82.00   1.00   15.78    --   14.49  57.00   0.00   84
  2  \w     19.00  47.00   1.00   15.78    --  -13.48  19.00-150.00   28
  3  \w     12.00  51.00   1.00   15.78    --  -13.48  77.00-150.00   39
  4  \w    -34.00  -7.00   1.00   15.78    --  -13.48  19.00-150.00   27
  5  \w    -40.00 -14.00   1.00   15.78    --  -13.48  77.00-150.00   26
  6  \w    -81.00  13.00   1.00   15.78    --  -13.48 -77.00  90.00   94
  7  \w     -5.00  21.00   1.00   15.78    --  -13.48 -99.00 -30.00   26
  8  \w     46.00  83.00   1.00   15.78    --   14.49-178.00 -30.00   37
;
_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      0.0239475000
_diffrn_orient_matrix_UB_12      0.0476533000
_diffrn_orient_matrix_UB_13      0.0327829000
_diffrn_orient_matrix_UB_21      -0.0515250000
_diffrn_orient_matrix_UB_22      -0.0434129000
_diffrn_orient_matrix_UB_23      0.0169724000
_diffrn_orient_matrix_UB_31      0.0543502000
_diffrn_orient_matrix_UB_32      -0.0405960000
_diffrn_orient_matrix_UB_33      0.0045010000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12357
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.497
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         3.204
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82536
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0321P)^2^+0.9780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5277
_reflns_number_total             6193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0217_suppl.cif
_cod_data_source_block           lgz-6
_cod_database_code               8105593
_chemical_oxdiff_usercomment     'c h n o ZN'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 H5WA(H5WB)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35),
 C36(H36), C37(H37), C38(H38)
;