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_1518542
_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(H2 O), 2(C H6 N3), 0.6224(C10 H26 N2), 0.1888(C12 H30 N2), 0.1888(C12 H30 N2)'
_chemical_formula_sum            'C28.7552 H49.5104 N8 O14 S4'
_chemical_formula_weight         859.59
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                94.880(3)
_cell_angle_beta                 96.822(3)
_cell_angle_gamma                95.184(3)
_cell_formula_units_Z            1
_cell_length_a                   9.7673(3)
_cell_length_b                   9.8143(3)
_cell_length_c                   10.2046(4)
_cell_measurement_reflns_used    6434
_cell_measurement_temperature    175
_cell_measurement_theta_max      32.3350
_cell_measurement_theta_min      2.0870
_cell_volume                     962.76(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_details
;
  1 omega   -4.00   91.00   1.0000   42.4400
omega____ theta____ kappa____ phi______ frames
    -       26.1732   77.0000 -150.0000 95

  2 omega    6.00   68.00   1.0000   42.4400
omega____ theta____ kappa____ phi______ frames
    -       26.1732 -100.0000   30.0000 62

  3 omega    3.00   63.00   1.0000   42.4400
omega____ theta____ kappa____ phi______ frames
    -       26.1732   77.0000  -60.0000 60

  4 omega  -42.00   53.00   1.0000   42.4400
omega____ theta____ kappa____ phi______ frames
    -       26.1732  -77.0000   90.0000 95

  5 omega  -89.00   30.00   1.0000   42.4400
omega____ theta____ kappa____ phi______ frames
    -      -26.9544    0.0000   60.0000 119

  6 omega   -4.00   96.00   1.0000   42.4400
omega____ theta____ kappa____ phi______ frames
    -       26.1732   77.0000   60.0000 100

  7 omega  -43.00   30.00   1.0000   42.4400
omega____ theta____ kappa____ phi______ frames
    -       26.1732  -57.0000 -180.0000 73

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0134280000
_diffrn_orient_matrix_UB_12      0.0704381000
_diffrn_orient_matrix_UB_13      0.0242412000
_diffrn_orient_matrix_UB_21      0.0699076000
_diffrn_orient_matrix_UB_22      -0.0099463000
_diffrn_orient_matrix_UB_23      0.0212029000
_diffrn_orient_matrix_UB_31      0.0183709000
_diffrn_orient_matrix_UB_32      0.0159899000
_diffrn_orient_matrix_UB_33      -0.0625279000
_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  0.027
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14777
_diffrn_reflns_theta_full        27.702
_diffrn_reflns_theta_max         32.590
_diffrn_reflns_theta_min         2.019
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90587
_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    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             454.041
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.53
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9213
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         5557
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.0007593
_refine_ls_shift/su_mean         0.0000241
_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: 
 9.36 1.96 6.12 1.10 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0698
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0649
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                5557
_reflns_number_total             6345
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.44
_oxford_diffrn_Wilson_scale      0.02
_oxford_refine_ls_r_factor_ref   0.0586
_oxford_refine_ls_scale          4.882(9)
_oxford_reflns_number_all        6345
_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        962.75(6)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               1518542
_cell_oxdiff_length_a            9.7673(3)
_cell_oxdiff_length_b            9.8143(3)
_cell_oxdiff_length_c            10.2046(4)
_cell_oxdiff_angle_alpha         94.880(3)
_cell_oxdiff_angle_beta          96.822(3)
_cell_oxdiff_angle_gamma         95.184(3)
_cell_oxdiff_volume              962.75(6)
_montpellier_reflns_maxres       0.66
_montpellier_reflns_completeness_maxres 90.46
_montpellier_reflns_redundancy_maxres 2.33
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE C(1,X'S, U'S) UNTIL N(22), 
CONT C(282,X'S,U[ISO],OCC) UNTIL C(232) 
EQUIVALENCE  C(231,U[ISO]) C(241,U[ISO]) 
CONT C(251,U[ISO]) C(261,U[ISO]) C(271,U[ISO]) 
EQUIVALENCE C(232,U[ISO]) C(242,U[ISO])  C(272,U[ISO]) C(282,U[ISO]) 
CONT C(252,U[ISO]) C(253,U[ISO]) C(262,U[ISO]) C(263,U[ISO]) 
EQUIVALENCE  C(231,OCC) C(241,OCC) C(251,OCC) C(261,OCC) C(271,OCC) 
CONT C(232,OCC) C(242,OCC)  C(272,OCC) C(282,OCC) 
CONT C(252,OCC) C(253,OCC) C(262,OCC) C(263,OCC) 
CONT H(2311,OCC) H(2312,OCC) H(2411,OCC) H(2412,OCC) 
CONT H(2511,OCC) H(2512,OCC) H(2611,OCC) H(2612,OCC) 
CONT H(2711,OCC) H(2712,OCC) 
CONT H(2321,OCC) H(2322,OCC) 
CONT  H(2421,OCC) H(2422,OCC)  H(2423,OCC) H(2424,OCC) 
CONT H(2521,OCC) H(2522,OCC) H(2531,OCC) H(2532,OCC) 
CONT H(2621,OCC) H(2622,OCC) H(2631,OCC) H(2632,OCC) 
CONT  H(2721,OCC) H(2722,OCC)  H(2723,OCC) H(2724,OCC)
CONT  H(2821,OCC) H(2822,OCC) 
WEIGHT -1 C(232,OCC) C(242,OCC)  C(272,OCC) C(282,OCC)
CONT H(2321,OCC) H(2322,OCC) H(2821,OCC) H(2822,OCC) 
WEIGHT -0.50 C(252,OCC) C(253,OCC) C(262,OCC) C(263,OCC) 
CONT  H(2421,OCC) H(2422,OCC)  H(2423,OCC) H(2424,OCC) 
CONT H(2721,OCC) H(2722,OCC)  H(2723,OCC) H(2724,OCC)
CONT H(2621,OCC) H(2622,OCC) H(2631,OCC) H(2632,OCC) 
CONT H(2521,OCC) H(2522,OCC) H(2531,OCC) H(2532,OCC) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE N   (  17,X'S) H   ( 172,X'S) H   ( 171,X'S) 
RIDE N   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) 
RIDE N   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) 
RIDE O   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (   232,X'S) H   (  2321,X'S)  H   (  2322,X'S) 
RIDE C   (   242,X'S) H(2421,X'S)  H(2422,X'S) H(2423,X'S) H(2424,X'S) 
RIDE C   (   252,X'S) H   (  2521,X'S)  H   (  2522,X'S) 
RIDE C   (   253,X'S) H   (  2531,X'S)  H   (  2532,X'S) 
RIDE C   (   262,X'S) H   (  2621,X'S)  H   (  2622,X'S) 
RIDE C   (   263,X'S) H   (  2631,X'S)  H   (  2632,X'S) 
RIDE C   (   272,X'S) H(2721,X'S)  H(2722,X'S) H(2723,X'S) H(2724,X'S) 
RIDE C   (   282,X'S) H   (  2821,X'S)  H   (  2822,X'S) 
RIDE C   (   231,X'S) H   (  2311,X'S)  H   (  2312,X'S) 
RIDE C   (   241,X'S) H   (  2411,X'S)  H   (  2412,X'S) 
RIDE C   (   251,X'S) H   (  2511,X'S)  H   (  2512,X'S) 
RIDE C   (   261,X'S) H   (  2611,X'S)  H   (  2612,X'S) 
RIDE C   (   271,X'S) H   (  2711,X'S)  H   (  2712,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
DIST 1.5,0.03=C(232) TO C(242), C(242) TO C(252), C(242) TO C(253), 
CONT C(252) TO C(262), C(253) TO C(263), C(262) TO C(272), C(263) TO C(272), 
CONT C(272) TO C(282), N(22) TO C(232) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
LIMIT      0.1000000 C(232,X) 
LIMIT      0.1000000 C(232,Y)
LIMIT      0.1000000 C(232,Z) 
LIMIT      0.01000000 OCC 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;