Supercooling Behavior and Dipole-Glass-like Relaxation in a Three-Dimensional Water Framework.
Huang, Rui-Kang; Wang, Sha-Sha; Liu, De-Xuan; Li, Xin; Song, Jian-Ming; Xia, Yuan-Hua; Zhou, Dong-Dong; Huang, Jin; Zhang, Wei-Xiong; Chen, Xiao-Ming; Journal of the American Chemical Society 141 (2019) 5645–5649; doi:10.1021/jacs.9b01866

data_4128411
_publ_section_title
;
 Supercooling Behavior and Dipole-Glass-like Relaxation in a
 Three-Dimensional Water Framework.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5645
_journal_page_last               5649
_journal_paper_doi               10.1021/jacs.9b01866
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C11 H3 F6 N6, C F3, 7(H2 O)'
_chemical_formula_sum            'C12 H17 F9 N6 O7'
_chemical_formula_weight         528.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2b 2ac'
_space_group_name_H-M_alt        'P c n b'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2019-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.283(3)
_cell_length_b                   7.7820(16)
_cell_length_c                   20.867(4)
_cell_measurement_reflns_used    11890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1886
_cell_measurement_theta_min      0.3739
_cell_volume                     1994.6(7)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_details
' 2.00 degrees, 115.6 sec, detector distance 115.00 mm'
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6525
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            11050
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        23.048
_diffrn_reflns_theta_max         31.158
_diffrn_reflns_theta_min         1.792
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_description       needle
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.041(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3656
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0791P)^2^+0.7236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3416
_reflns_number_total             3656
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            FFP.cif
_cod_data_source_block           ffp
_cod_database_code               4128411
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.992
_olex2_refinement_description
;
1. Restrained distances
 H2A-H2B \\sim H2A-H2C \\sim H2B-H2C
 with sigma of 0.04
 O2-H2A \\sim O2-H2B \\sim O2-H2C \\sim O2-H2D
 with sigma of 0.02
 H3A-H3B \\sim H3A-H3C \\sim H3A-H3D \\sim H3B-H3C \\sim H3B-H3D \\sim H3A-H3D
\\sim H3C-H3D
 with sigma of 0.04
 O3-H3A \\sim O3-H3B \\sim O3-H3C \\sim O3-H3D
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
F2' \\sim F2 \\sim F1' \\sim F1 \\sim F3' \\sim F3: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
H3D \\sim H3A \\sim H3B \\sim H3C \\sim H2D \\sim H2A \\sim H2B \\sim H2C \\sim
H4B \\sim H4A \\sim H1D \\sim H1A \\sim H1B \\sim H1C: within 6.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(F5')=Sof(F6')=Sof(F4')=1-FVAR(1)
 Sof(F5)=Sof(F6)=Sof(F4)=FVAR(1)
 Fixed Sof: F1(0.25) F3(0.25) F2(0.25) F2'(0.25) F3'(0.25) F1'(0.25) H3(0.5)
 H2(0.5) H1(0.5) H2A(0.5) H3A(0.5) H1A(0.5) H4A(0.5) H3B(0.5) H2B(0.5) H1B(0.5)
 H1C(0.5) H2C(0.5) H1D(0.5) H3C(0.5) H3D(0.5) H4B(0.5) H2D(0.5)
;
_shelx_res_checksum              79089
_shelx_hkl_checksum              7755
_olex2_submission_special_instructions 'No special instructions were received'