Measurement of Electric Fields Experienced by Urea Guest Molecules in the 18-Crown-6/Urea (1:5) Host-Guest Complex: An Experimental Reference Point for Electric-Field-Assisted Catalysis.
Shi, Ming W.; Thomas, Sajesh P.; Hathwar, Venkatesha R.; Edwards, Alison J.; Piltz, Ross O.; Jayatilaka, Dylan; Koutsantonis, George A.; Overgaard, Jacob; Nishibori, Eiji; Iversen, Bo B.; Spackman, Mark A.; Journal of the American Chemical Society 141 (2019) 3965–3976; doi:10.1021/jacs.8b12927

data_4128535
_publ_section_title
;
 Measurement of Electric Fields Experienced by Urea Guest Molecules in the
 18-Crown-6/Urea (1:5) Host-Guest Complex: An Experimental Reference Point
 for Electric-Field-Assisted Catalysis.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3965
_journal_page_last               3976
_journal_paper_doi               10.1021/jacs.8b12927
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C17 H44 N10 O11'
_chemical_formula_sum            'C17 H44 N10 O11'
_chemical_formula_weight         564.60
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     geom
_audit_creation_date             2016-03-31
_audit_creation_method           'CRYSTALS_ver_14.61 + LaueG software'
_cell_angle_alpha                90
_cell_angle_beta                 108.527(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8250(3)
_cell_length_b                   8.25020(10)
_cell_length_c                   20.6233(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    30
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2875.68(16)
_computing_cell_refinement       'LaueG (Piltz, 2018)'
_computing_data_collection       'MAATEL/ANSTO control program'
_computing_data_reduction
'argonne_boxes (Wilkinson et al., 1988) & LaueG (Piltz, 2018)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Known from Xray'
_diffrn_ambient_temperature      30
_diffrn_measured_fraction_theta_full 0.824
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_details      '41 images, exposure time 5000s '
_diffrn_measurement_device       'Laue image-plate diffractometer'
_diffrn_measurement_device_type  KOALA
_diffrn_measurement_method       Laue
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.85
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_unetI/netI     0.1019
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            194702
_diffrn_reflns_reduction_process 'LaueG (Piltz, 2018)'
_diffrn_reflns_resolution_max    1.67
_diffrn_reflns_theta_full        71.23
_diffrn_reflns_theta_max         71.33
_diffrn_source                   'nuclear reactor'
_diffrn_source_details           'thermal neutrons, supermirror guides'
_diffrn_source_type              'OPAL reactor, ANSTO, Lucas Heights, Australia'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             396
_exptl_crystal_size_max          1.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.6
_refine_diff_density_max         1.81
_refine_diff_density_min         -1.95
_refine_ls_extinction_coef       12.516
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9312
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         7840
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.0006744
_refine_ls_shift/su_mean         0.0000475
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 5.14 -1.25 2.33 1.80 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0533
_refine_ls_wR_factor_gt          0.0379
_refine_ls_wR_factor_ref         0.0371
_reflns_limit_h_max              28
_reflns_limit_h_min              -29
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                8730
_reflns_number_total             11494
_reflns_threshold_expression     >3sigma(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0499
_oxford_refine_ls_scale          0.5190(5)
_oxford_reflns_number_all        11078
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'shelx in E:\Crystal30_alison\spa At 11:28 on'
_cod_data_source_file            ja8b12927_si_002.cif
_cod_data_source_block           global
_cod_original_cell_volume        2875.68(6)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4128535