Crystal structure of catena-poly[(μ2-isophthalato-κ2 O:O′)-(2,5-di(pyrazin-2-yl)-4,4′-bipyridine-κ3 N,N′,N′′)zinc(II)] — water (2/5), C26H21N6O6.5Zn
Wang, Yu-Fang; Zhang, Yong-Hua; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 1043–1045; doi:10.1515/ncrs-2019-0250

data_8105932
_publ_section_title
;
 Crystal structure of catena-poly[(\m2-isophthalato-\k2
 O:O&#x2032;)-(2,5-di(pyrazin-2-yl)-4,4&#x2032;-bipyridine-\k3
 N,N&#x2032;,N&#x2032;&#x2032;)zinc(II)] --- water (2/5), C26H21N6O6.5Zn
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1043
_journal_page_last               1045
_journal_paper_doi               10.1515/ncrs-2019-0250
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C26 H16 N6 O4 Zn, 2.5(H2 O)'
_chemical_formula_sum            'C26 H21 N6 O6.5 Zn'
_chemical_formula_weight         586.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 99.5396(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.3123(3)
_cell_length_b                   8.97463(15)
_cell_length_c                   30.1437(5)
_cell_measurement_reflns_used    20949
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5650
_cell_measurement_theta_min      3.8600
_cell_volume                     4885.49(14)
_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 0.998
_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    -43.00  52.00   1.00   10.00    --  -15.84  77.00-150.00   95
  2  \w    -10.00  84.00   1.00   10.00    --   16.93  77.00  90.00   94
  3  \w      0.00  84.00   1.00   10.00    --   16.93  57.00  30.00   84
  4  \w    -51.00  44.00   1.00   10.00    --   16.93 -77.00-180.00   95
  5  \w    -10.00  84.00   1.00   10.00    --   16.93  77.00 -60.00   94
  6  \w      0.00  84.00   1.00   10.00    --   16.93  57.00-150.00   84
  7  \w     35.00  89.00   1.00   10.00    --   16.93 178.00-180.00   54
  8  \w    -20.00  56.00   1.00   10.00    --   16.93 -99.00 -60.00   76
  9  \w    -20.00  56.00   1.00   10.00    --   16.93 -99.00  60.00   76
 10  \w     34.00  90.00   1.00   10.00    --   16.93-178.00  90.00   56
 11  \w    -20.00  56.00   1.00   10.00    --   16.93 -99.00 150.00   76
 12  \w     -2.00  86.00   1.00   10.00    --   16.93  38.00 -60.00   88
;
_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      0.0217530000
_diffrn_orient_matrix_UB_12      0.0039994000
_diffrn_orient_matrix_UB_13      -0.0173575000
_diffrn_orient_matrix_UB_21      0.0296002000
_diffrn_orient_matrix_UB_22      -0.0359587000
_diffrn_orient_matrix_UB_23      0.0141493000
_diffrn_orient_matrix_UB_31      -0.0139160000
_diffrn_orient_matrix_UB_32      -0.0702747000
_diffrn_orient_matrix_UB_33      -0.0082274000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            45759
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.496
_diffrn_reflns_theta_min         3.249
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72026
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         4533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0168P)^2^+10.4065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4224
_reflns_number_total             4533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0250_suppl.cif
_cod_data_source_block           w102
_cod_original_cell_volume        4885.51(14)
_cod_original_formula_sum        'C26 H21 N6 O6.50 Zn'
_cod_database_code               8105932
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H2AA(0.5) H2AB(0.5)
3.a Free rotating group:
 O5(H5A,H5B), O2AA(H2AA,H2AB), O6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C1(H1), C2(H2), C3(H3), C17(H17), C18(H18), C8(H8), C6(H6),
 C11(H11), C12(H12), C13(H13), C14(H14), C25(H25), C24(H24), C23(H23), C21(H21)
;
_olex2_date_sample_data_collection 2018-06-07
_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 1.258
_oxdiff_exptl_absorpt_empirical_full_min 0.630