Salt-Excluding Artificial Water Channels Exhibiting Enhanced Dipolar Water and Proton Translocation.
Licsandru, Erol; Kocsis, Istvan; Shen, Yue-Xiao; Murail, Samuel; Legrand, Yves-Marie; van der Lee, Arie; Tsai, Daniel; Baaden, Marc; Kumar, Manish; Barboiu, Mihail; Journal of the American Chemical Society 138 (2016) 5403–5409; doi:10.1021/jacs.6b01811

data_4130276
_publ_section_title
;
 Salt-Excluding Artificial Water Channels Exhibiting Enhanced Dipolar
 Water and Proton Translocation.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5403
_journal_page_last               5409
_journal_paper_doi               10.1021/jacs.6b01811
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C14 H26 N4 O, 0.5(H2 O)'
_chemical_formula_sum            'C14 H27 N4 O1.5'
_chemical_formula_weight         275.39
_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_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 107.482(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.180(2)
_cell_length_b                   4.5911(2)
_cell_length_c                   23.9057(14)
_cell_measurement_reflns_used    1316
_cell_measurement_temperature    175
_cell_measurement_theta_max      44.9160
_cell_measurement_theta_min      3.0390
_cell_volume                     3159.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      175
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0143
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -67.00  -20.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  150.0000  110.0000 47

  2 omega  -26.00   16.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -150.0000 42

  3 omega   43.00  108.00   1.0000  475.0000
omega____ theta____ kappa____ phi______ frames
    -       52.8885   57.0000   90.0000 65

  4 omega   24.00   91.00   1.0000  475.0000
omega____ theta____ kappa____ phi______ frames
    -       52.8885  -99.0000   30.0000 67

  5 omega   57.00   86.00   1.0000  475.0000
omega____ theta____ kappa____ phi______ frames
    -       52.8885   57.0000  -30.0000 29

  6 omega   -4.00   80.00   1.0000  475.0000
omega____ theta____ kappa____ phi______ frames
    -       52.8885  -99.0000  -60.0000 84

  7 omega  -13.00   69.00   1.0000  475.0000
omega____ theta____ kappa____ phi______ frames
    -       52.8885  -19.0000   90.0000 82

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0014680000
_diffrn_orient_matrix_UB_12      0.3354052000
_diffrn_orient_matrix_UB_13      0.0012353000
_diffrn_orient_matrix_UB_21      0.0532717000
_diffrn_orient_matrix_UB_22      -0.0096105000
_diffrn_orient_matrix_UB_23      0.0259117000
_diffrn_orient_matrix_UB_31      0.0047688000
_diffrn_orient_matrix_UB_32      0.0025836000
_diffrn_orient_matrix_UB_33      -0.0623943000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4509
_diffrn_reflns_theta_full        44.068
_diffrn_reflns_theta_max         44.967
_diffrn_reflns_theta_min         3.070
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelets
_exptl_crystal_F_000             1207.989
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9692
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         2085
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.1115
_refine_ls_shift/su_max          0.0003261
_refine_ls_shift/su_mean         0.0000604
_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: 
 30.1 36.0 27.9 13.4 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0916
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0831
_reflns_limit_h_max              26
_reflns_limit_h_min              -27
_reflns_limit_k_max              4
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2085
_reflns_number_total             2516
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.1115
_oxford_refine_ls_scale          1.728(9)
_oxford_reflns_number_all        2516
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ja6b01811_si_005.cif
_cod_data_source_block           1
_cod_depositor_comments
;

2020-07-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        3159.33(19)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_moiety     '2(C14 H26 N4 O), H2 O'
_cod_original_formula_sum        'C28 H54 N8 O3'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     550.79
_cod_database_code               4130276
_cell_oxdiff_length_a            30.183(3)
_cell_oxdiff_length_b            4.5911(3)
_cell_oxdiff_length_c            23.8996(15)
_cell_oxdiff_angle_alpha         90.018(5)
_cell_oxdiff_angle_beta          107.458(7)
_cell_oxdiff_angle_gamma         89.972(7)
_cell_oxdiff_volume              3159.3(4)
_montpellier_reflns_maxres       1.09
_montpellier_reflns_completeness_maxres 98.74
_montpellier_reflns_redundancy_maxres 1.75