Crystal structure of catena-poly[diaqua-(μ2-1,2-bis(4-pyridinyl)ethyane-κ2 N:N′)-(μ2–pyridazine-4,5-dicarboxylato-κ2 O:O′)]dizinc(II) dihydrate, C12H12ZnN3O6
Feng-Yang, Ju; Ke-Xin, Ding; Fang, Liu; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 567–569; doi:10.1515/ncrs-2018-0565

data_8105781
_publ_section_title
;
 Crystal structure of
 catena-poly[diaqua-(\m2-1,2-bis(4-pyridinyl)ethyane-\k2
 N:N&#x2032;)-(\m2--pyridazine-4,5-dicarboxylato-\k2
 O:O&#x2032;)]dizinc(II) dihydrate, C12H12ZnN3O6
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              567
_journal_page_last               569
_journal_paper_doi               10.1515/ncrs-2018-0565
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C12 H10 N3 O5 Zn, H2 O'
_chemical_formula_sum            'C12 H12 N3 O6 Zn'
_chemical_formula_weight         359.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 107.899(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.6153(6)
_cell_length_b                   6.6922(2)
_cell_length_c                   24.1330(9)
_cell_measurement_reflns_used    7802
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9270
_cell_measurement_theta_min      3.8950
_cell_volume                     2707.23(17)
_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 0.891
_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    -86.00 -35.00   1.00    7.12    --  -13.80-178.00-120.00   51
  2  \w    -41.00  54.00   1.00    7.12    --  -13.80  77.00-150.00   95
  3  \w    -20.00  25.00   1.00    7.12    --  -13.80 -99.00 -30.00   45
  4  \w    -83.00   5.00   1.00    7.12    --  -13.80 -38.00 -90.00   88
  5  \w    -31.00  53.00   1.00    7.12    --  -13.80  57.00-180.00   84
  6  \w    -81.00  13.00   1.00    7.12    --  -13.80 -77.00  90.00   94
;
_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      -0.0254589000
_diffrn_orient_matrix_UB_12      0.0062925000
_diffrn_orient_matrix_UB_13      -0.0291416000
_diffrn_orient_matrix_UB_21      0.0332859000
_diffrn_orient_matrix_UB_22      0.0234939000
_diffrn_orient_matrix_UB_23      -0.0094380000
_diffrn_orient_matrix_UB_31      0.0060260000
_diffrn_orient_matrix_UB_32      -0.1031666000
_diffrn_orient_matrix_UB_33      -0.0039382000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            12623
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         3.278
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55656
_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    1.765
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0353P)^2^+2.3754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2649
_reflns_number_total             2990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0565_suppl.cif
_cod_data_source_block           jfy-41
_cod_original_cell_volume        2707.22(17)
_cod_database_code               8105781
_shelx_estimated_absorpt_t_max   0.697
_shelx_estimated_absorpt_t_min   0.556
_reflns_odcompleteness_completeness 99.70
_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 Riding coordinates:
 O2W(H2WA,H2WB)
2.b Rotating group:
 O1W(H1WA,H1WB)
2.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11)
;
_olex2_date_sample_data_collection 2018-09-10
_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 1.391
_oxdiff_exptl_absorpt_empirical_full_min 0.577