Smart urea ionic co-crystals with enhanced urease inhibition activity for improved nitrogen cycle management.
Casali, Lucia; Mazzei, Luca; Shemchuk, Oleksii; Honer, Kenneth; Grepioni, Fabrizia; Ciurli, Stefano; Braga, Dario; Baltrusaitis, Jonas; Chemical communications (Cambridge, England) 54 (2018) 7637–7640; doi:10.1039/c8cc03777a

data_7121838
_publ_section_title
;
 Smart urea ionic co-crystals with enhanced urease inhibition activity for
 improved nitrogen cycle management.
;
_journal_issue                   55
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7637
_journal_page_last               7640
_journal_paper_doi               10.1039/c8cc03777a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C H4 Cl3 K N2 O Zn'
_chemical_formula_sum            'C H4 Cl3 K N2 O Zn'
_chemical_formula_weight         270.88
_chemical_melting_point          415
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-03 deposited with the CCDC.
2018-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.089(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4220(6)
_cell_length_b                   13.5530(10)
_cell_length_c                   8.4219(5)
_cell_measurement_reflns_used    2604
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8330
_cell_measurement_theta_min      5.5000
_cell_volume                     846.60(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.796
_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    -79.00  -5.00   1.00   32.50    --  -16.52 137.00 -37.74   74
  2  \w    -16.00  20.00   1.00   32.50    --  -16.52 -99.00 -30.00   36
  3  \w    -68.00   5.00   1.00   32.50    --  -16.52 119.00  64.63   73
  4  \w    -34.00  52.00   1.00   32.50    --  -16.52  57.00-150.00   86
  5  \w    -85.00 -23.00   1.00   32.50    --  -16.52 -57.00  60.00   62
  6  \w    -85.00   1.00   1.00   32.50    --  -16.52 -77.00 150.00   86
  7  \w     -2.00  88.00   1.00   32.50    --   17.61  38.00   0.00   90
  8  \w    -17.00  58.00   1.00   32.50    --   17.61 -99.00 -60.00   75
  9  \w     -5.00  87.00   1.00   32.50    --   17.61  38.00 -90.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0948538000
_diffrn_orient_matrix_UB_12      0.0065162000
_diffrn_orient_matrix_UB_13      -0.0006657000
_diffrn_orient_matrix_UB_21      -0.0008890000
_diffrn_orient_matrix_UB_22      -0.0152711000
_diffrn_orient_matrix_UB_23      0.0805309000
_diffrn_orient_matrix_UB_31      0.0121682000
_diffrn_orient_matrix_UB_32      0.0496333000
_diffrn_orient_matrix_UB_33      0.0248179000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.894
_diffrn_reflns_Laue_measured_fraction_max 0.796
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9911
_diffrn_reflns_point_group_measured_fraction_full 0.894
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.442
_diffrn_reflns_theta_min         3.595
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.266
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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    2.125
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.600
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.600
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0305
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1326
_reflns_number_total             1867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03777a2.cif
_cod_data_source_block           twin_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7121837--7121838.cif.'
_cod_database_code               7121838
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.567
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2.a X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
;
_shelx_res_checksum              44141
_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 2.948
_oxdiff_exptl_absorpt_empirical_full_min 0.898
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by -179.9939\% 
 around [1.00 -0.00 -0.04] (reciprocal) or [1.00 -0.00 0.00] (direct)
;