Crystal structure of tetraaqua-bis[6-(1H-imidazol-1-yl-κN)nicotinato]zinc(II), C18H20N6O8Zn
Li, Zhao-Hao; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 273–274; doi:10.1515/ncrs-2017-0271

data_8106123
_publ_section_title
;
 Crystal structure of
 tetraaqua-bis[6-(1H-imidazol-1-yl-\kN)nicotinato]zinc(II), C18H20N6O8Zn
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              273
_journal_page_last               274
_journal_paper_doi               10.1515/ncrs-2017-0271
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C18 H20 N6 O8 Zn'
_chemical_formula_sum            'C18 H20 N6 O8 Zn'
_chemical_formula_weight         513.77
_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                78.536(10)
_cell_angle_beta                 86.677(9)
_cell_angle_gamma                72.340(9)
_cell_formula_units_Z            1
_cell_length_a                   6.2576(6)
_cell_length_b                   6.9645(8)
_cell_length_c                   12.1262(15)
_cell_measurement_reflns_used    2117
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.6070
_cell_measurement_theta_min      3.9880
_cell_volume                     493.52(10)
_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_environment      air
_diffrn_ambient_temperature      291(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.980
_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    -80.00  14.00   1.00   30.00    --  -12.53 -77.00  60.00   94
  2  \w    -39.00  55.00   1.00   30.00    --  -12.53  77.00-180.00   94
  3  \w    -20.00  26.00   1.00   30.00    --  -12.53 -99.00  90.00   46
  4  \w    -54.00  40.00   1.00   30.00    --   13.55 -77.00 -60.00   94
  5  \w    -16.00  85.00   1.00   30.00    --   13.55  19.00  30.00  101
  6  \w     34.00  86.00   1.00   30.00    --   13.55-178.00 -60.00   52
  7  \w    -42.00 -17.00   1.00   30.00    --  -12.53  19.00  90.00   25
;
_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      -0.1171971000
_diffrn_orient_matrix_UB_12      0.0485175000
_diffrn_orient_matrix_UB_13      0.0016971000
_diffrn_orient_matrix_UB_21      0.0116169000
_diffrn_orient_matrix_UB_22      0.0192217000
_diffrn_orient_matrix_UB_23      0.0542915000
_diffrn_orient_matrix_UB_31      0.0167409000
_diffrn_orient_matrix_UB_32      0.0955530000
_diffrn_orient_matrix_UB_33      -0.0247340000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4947
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.489
_diffrn_reflns_theta_min         3.417
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.308
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62947
_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_colour_primary    colourless
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       block
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         1812
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+1.0200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1290
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1569
_reflns_number_total             1812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0271_suppl.cif
_cod_data_source_block           3
_cod_database_code               8106123
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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. Rigid bond restraints
 N3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Rotating group:
 O4(H3W,H4W), O3(H2W,H1W)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C2(H2), C1(H1), C6(H6), C8(H8)
;
_shelx_res_checksum              16288
_shelx_hkl_checksum              67166
_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 1.685
_oxdiff_exptl_absorpt_empirical_full_min 0.629