Crystal structure of diaqua-bis(5-carboxy-1-methyl-1H-imidazole-4-carboxylato-κ2 N,O)zinc(II), C12H14N4O10Zn
Xiao-Ling, Li; Ru-Meng, Zhang; Li, Liu; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 833–834; doi:10.1515/ncrs-2018-0042

data_8106315
_publ_section_title
;
 Crystal structure of
 diaqua-bis(5-carboxy-1-methyl-1H-imidazole-4-carboxylato-\k2
 N,O)zinc(II), C12H14N4O10Zn
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              833
_journal_page_last               834
_journal_paper_doi               10.1515/ncrs-2018-0042
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C6 H7 N2 O5 Zn0.5'
_chemical_formula_sum            'C6 H7 N2 O5 Zn0.5'
_chemical_formula_weight         219.82
_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
_cell_angle_alpha                90
_cell_angle_beta                 95.040(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.0277(4)
_cell_length_b                   12.0102(5)
_cell_length_c                   15.3939(5)
_cell_measurement_reflns_used    9629
_cell_measurement_temperature    292.04(10)
_cell_measurement_theta_max      26.4920
_cell_measurement_theta_min      3.9920
_cell_volume                     1662.62(11)
_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      292.04(10)
_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     -6.00  78.00   1.00    9.59    --   10.64  57.00  90.00   84
  2  \w    -58.00  30.00   1.00    9.59    --   10.64 -38.00 150.00   88
  3  \w     -6.00  78.00   1.00    9.59    --   10.64  57.00 -30.00   84
  4  \w    -20.00  50.00   1.00    9.59    --   10.64 -99.00 120.00   70
  5  \w    -20.00  50.00   1.00    9.59    --   10.64 -99.00 -90.00   70
  6  \w    -20.00  50.00   1.00    9.59    --   10.64 -99.00   0.00   70
  7  \w     -6.00  78.00   1.00    9.59    --   10.64  57.00-180.00   84
  8  \w     -6.00  78.00   1.00    9.59    --   10.64  57.00 -90.00   84
  9  \w    -20.00  29.00   1.00    9.59    --   -9.62 -99.00 -60.00   49
 10  \w    -20.00  50.00   1.00    9.59    --   10.64 -99.00 -60.00   70
 11  \w    -20.00  50.00   1.00    9.59    --   10.64 -99.00-180.00   70
 12  \w    -57.00 -24.00   1.00    9.59    --   10.64 -57.00  60.00   33
 13  \w    -20.00  50.00   1.00    9.59    --   10.64 -99.00  60.00   70
;
_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      0.0292719000
_diffrn_orient_matrix_UB_12      0.0538151000
_diffrn_orient_matrix_UB_13      -0.0066243000
_diffrn_orient_matrix_UB_21      0.0729898000
_diffrn_orient_matrix_UB_22      -0.0223740000
_diffrn_orient_matrix_UB_23      0.0032226000
_diffrn_orient_matrix_UB_31      -0.0060676000
_diffrn_orient_matrix_UB_32      -0.0094006000
_diffrn_orient_matrix_UB_33      -0.0456818000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15049
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.393
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.542
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67436
_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    1.756
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0257P)^2^+2.4887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1415
_reflns_number_total             1453
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0042_suppl.cif
_cod_data_source_block           lgz
_cod_original_formula_sum        'C6 H7 N2 O5 Zn0.50'
_cod_database_code               8106315
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O1W(H1WA,H1WB), O3(H3)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3A)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              93168
_shelx_hkl_checksum              13867
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2017-09-20
_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 1.331
_oxdiff_exptl_absorpt_empirical_full_min 0.699