Adaptive binding and selection of compressed 1,ω-diammonium-alkanes via molecular encapsulation in water
Dumitrescu, Dan; Legrand, Yves-Marie; Petit, Eddy; van der Lee, Arie; Barboiu, Mihail; Chem. Sci. 6 (2015) 2079–; doi:10.1039/C4SC03945A

data_1518541
_publ_section_title
;
 Adaptive binding and selection of compressed 1,\w-diammonium-alkanes via
 molecular encapsulation in water
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              2079
_journal_paper_doi               10.1039/C4SC03945A
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C16 H6 O12 S4, 2(C10 H26 N2), 4(H2 O)'
_chemical_formula_sum            'C36 H66 N4 O16 S4'
_chemical_formula_weight         939.21
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2yc'
_symmetry_space_group_name_H-M   'I 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_update_record
;
2014-12-19 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.758(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4827(5)
_cell_length_b                   7.7013(2)
_cell_length_c                   30.1416(7)
_cell_measurement_reflns_used    5367
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.8650
_cell_measurement_theta_min      2.1370
_cell_volume                     4427.61(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details
;
  1 omega   23.00   56.00   1.0000   91.0300
omega____ theta____ kappa____ phi______ frames
    -       17.7668 -100.0000   90.0000 33

  2 omega  -18.00   88.00   1.0000   91.0300
omega____ theta____ kappa____ phi______ frames
    -       17.7668   19.0000  150.0000 106

  3 omega  -55.00   59.00   1.0000   91.0300
omega____ theta____ kappa____ phi______ frames
    -       17.7668  -19.0000  150.0000 114

  4 omega  -12.00   22.00   1.0000   91.0300
omega____ theta____ kappa____ phi______ frames
    -       17.7668   77.0000 -120.0000 34

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0148556000
_diffrn_orient_matrix_UB_12      0.0567455000
_diffrn_orient_matrix_UB_13      -0.0140152000
_diffrn_orient_matrix_UB_21      -0.0336191000
_diffrn_orient_matrix_UB_22      0.0127778000
_diffrn_orient_matrix_UB_23      -0.0139599000
_diffrn_orient_matrix_UB_31      -0.0057976000
_diffrn_orient_matrix_UB_32      0.0713580000
_diffrn_orient_matrix_UB_33      0.0136454000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            12680
_diffrn_reflns_theta_full        25.281
_diffrn_reflns_theta_max         29.059
_diffrn_reflns_theta_min         2.135
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.62
_refine_diff_density_min         -0.64
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0486
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4256
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.0009738
_refine_ls_shift/su_mean         0.0000676
_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: 
 18.1 17.9 17.5 6.36 1.75 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0830
_refine_ls_wR_factor_gt          0.0767
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_reflns_limit_h_max              23
_reflns_limit_h_min              -25
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              41
_reflns_limit_l_min              0
_reflns_number_gt                4256
_reflns_number_total             5162
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.81
_oxford_diffrn_Wilson_scale      0.42
_oxford_refine_ls_r_factor_ref   0.0746
_oxford_refine_ls_scale          1.194(4)
_oxford_reflns_number_all        5162
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c4sc03945a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1518540--1518542.cif.'
_cod_original_cell_volume        4427.63(11)
_cod_original_sg_symbol_H-M      'I 2/c '
_cod_database_code               1518541
_cell_oxdiff_length_a            19.4702(9)
_cell_oxdiff_length_b            7.7046(3)
_cell_oxdiff_length_c            30.1459(14)
_cell_oxdiff_angle_alpha         90.001(3)
_cell_oxdiff_angle_beta          101.739(4)
_cell_oxdiff_angle_gamma         89.994(4)
_cell_oxdiff_volume              4427.6(3)
_montpellier_reflns_maxres       0.73
_montpellier_reflns_completeness_maxres 87.50
_montpellier_reflns_redundancy_maxres 2.40