Confined water in imidazolium based ionic liquids: a supramolecular guest@host complex case.
Zanatta, Marcileia; Girard, Anne-Lise; Marin, Graciane; Ebeling, Gunter; Dos Santos, Francisco P.; Valsecchi, Chiara; Stassen, Hubert; Livotto, Paolo R.; Lewis, William; Dupont, Jairton; Physical chemistry chemical physics : PCCP 18 (2016) 18297–18304; doi:10.1039/c6cp03112a

data_7225656
_publ_section_title
;
 Confined water in imidazolium based ionic liquids: a supramolecular
 guest@host complex case.
;
_journal_issue                   27
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              18297
_journal_page_last               18304
_journal_paper_doi               10.1039/c6cp03112a
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C6 H11 N2, C3 H3 N2, H2 O'
_chemical_formula_sum            'C9 H16 N4 O'
_chemical_formula_weight         196.26
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2016-04-04 deposited with the CCDC.
2016-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.725(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3864(4)
_cell_length_b                   12.0203(7)
_cell_length_c                   12.5938(7)
_cell_measurement_reflns_used    2665
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.9650
_cell_measurement_theta_min      3.7680
_cell_volume                     1086.23(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
  1 omega   71.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -45.0000    0.0000 27

  2 omega   33.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -30.0000    0.0000 58

  3 omega   29.00   56.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9402 -133.0000  -77.0000 27

  4 omega   38.00  121.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822 -125.0000 -150.0000 83

  5 omega   85.00  175.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822   15.0000 -180.0000 90

  6 omega   76.00  104.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822   77.0000  120.0000 28

  7 omega  121.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822   77.0000  120.0000 56

  8 omega   96.00  157.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  125.0000  150.0000 61

  9 omega   37.00   96.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -45.0000  150.0000 59

 10 omega -109.00  -22.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000  150.0000 87

 11 omega -111.00  -23.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000   30.0000 88
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      -0.0653974000
_diffrn_orient_matrix_UB_12      0.0599118000
_diffrn_orient_matrix_UB_13      0.0924425000
_diffrn_orient_matrix_UB_21      -0.1438357000
_diffrn_orient_matrix_UB_22      0.0659997000
_diffrn_orient_matrix_UB_23      -0.0855514000
_diffrn_orient_matrix_UB_31      -0.1452698000
_diffrn_orient_matrix_UB_32      -0.0920833000
_diffrn_orient_matrix_UB_33      -0.0010436000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4439
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.873
_diffrn_reflns_theta_min         5.158
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.9416
_exptl_crystal_size_mid          0.63
_exptl_crystal_size_min          0.5186
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0928P)^2^+0.2170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1988
_reflns_number_total             2149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cp03112a2.cif
_cod_data_source_block           ojdula
_cod_depositor_comments          'Adding full bibliography for 7225656.cif.'
_cod_original_cell_volume        1086.24(11)
_cod_database_code               7225656
_nottingham_internal_coll_name   OJDULA
_nottingham_internal_coll_number 14056
_nottingham_internal_coll_client /JDU
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time 2.0000
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pczwl
_nottingham_internal_coll_date   09/10/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 10/10/2014
_nottingham_internal_process_user pczwl
_nottingham_internal_solution_date 10/10/2014
_nottingham_internal_solution_user pczwl
_nottingham_internal_refinement_date 14/10/2014
_nottingham_internal_refinement_user pczwl
_nottingham_internal_validation_date 14/10/2014
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 14/10/2014
_chemical_oxdiff_formula         'C9 H16 N4 O'
_chemical_oxdiff_usercomment
'OJDULA #14056 SN-320 IN FOMBLIN FILM ON A MICROMOUNT FOR /JDU'
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C10(H10), C12(H12), C13(H13)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              69036
_shelx_shelxl_version_number     2014/7
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'