Progressive compression of 1,omega-diammonium-alkanes inside a rigid crystalline molecular cage
Dan Dumitrescu; Yves-Marie Legrand; Eddy Petit; Arie van der Lee; Mihail Barboiu; Chem.Commun. 50 (2014) 14086–; doi:10.1039/C4cc03866E

data_7115930
_publ_section_title
;
 Progressive compression of 1,omega-diammonium-alkanes inside a rigid
 crystalline molecular cage
;
_journal_name_full               Chem.Commun.
_journal_page_first              14086
_journal_paper_doi               10.1039/C4cc03866E
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety
'C12 H30 N2, C16 H6 O12 S4, 2(C H6 N3), 2(H2 O)'
_chemical_formula_sum            'C30 H52 N8 O14 S4'
_chemical_formula_weight         877.08
_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
_cell_angle_alpha                94.489(3)
_cell_angle_beta                 97.927(3)
_cell_angle_gamma                95.090(3)
_cell_formula_units_Z            1
_cell_length_a                   9.7985(3)
_cell_length_b                   9.8928(3)
_cell_length_c                   10.2589(4)
_cell_measurement_reflns_used    11991
_cell_measurement_temperature    175
_cell_measurement_theta_max      32.7610
_cell_measurement_theta_min      2.0400
_cell_volume                     976.92(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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 0.996
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details
;
  1 omega  -42.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955    0.0000  -60.0000 134

  2 omega  -60.00  -11.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330   92.0000 -124.0000 49

  3 omega  -92.00    1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330  -77.0000  -60.0000 93

  4 omega  -31.00    2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330  -77.0000  120.0000 33

  5 omega  -60.00   -3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330   92.0000   55.0000 57

  6 omega  -91.00  -21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330  -38.0000   90.0000 70

  7 omega   34.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955  179.0000 -120.0000 62

  8 omega   34.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955  179.0000   30.0000 62

  9 omega  -92.00   -8.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330  -57.0000  -30.0000 84

 10 omega  -92.00    2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330  -77.0000 -180.0000 94

 11 omega  -94.00   -6.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330  -38.0000    0.0000 88

 12 omega    7.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955   57.0000  150.0000 84

 13 omega  -25.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955  -99.0000 -120.0000 88

 14 omega  -43.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955  -57.0000   90.0000 84

 15 omega    7.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955   57.0000  -60.0000 84

 16 omega  -25.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955  -99.0000   30.0000 88

 17 omega  -25.00   50.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955  -99.0000  150.0000 75

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0185242000
_diffrn_orient_matrix_UB_12      -0.0073150000
_diffrn_orient_matrix_UB_13      -0.0644365000
_diffrn_orient_matrix_UB_21      -0.0099762000
_diffrn_orient_matrix_UB_22      -0.0719131000
_diffrn_orient_matrix_UB_23      -0.0001654000
_diffrn_orient_matrix_UB_31      -0.0703835000
_diffrn_orient_matrix_UB_32      0.0006634000
_diffrn_orient_matrix_UB_33      -0.0276089000
_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  0.038
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35243
_diffrn_reflns_theta_full        28.822
_diffrn_reflns_theta_max         32.752
_diffrn_reflns_theta_min         2.013
_exptl_absorpt_coefficient_mu    0.319
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             463.805
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.01
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0533
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5973
_refine_ls_number_restraints     199
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.0007422
_refine_ls_shift/su_mean         0.0000395
_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: 
 14.7 13.7 13.3 4.41 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0562
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0494
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              -15
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                5973
_reflns_number_total             6778
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.22
_oxford_diffrn_Wilson_scale      0.01
_oxford_refine_ls_r_factor_ref   0.0404
_oxford_refine_ls_scale          5.974(10)
_oxford_reflns_number_all        6778
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c4cc03866e2.cif
_cod_data_source_block           1d
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7115930
_cell_oxdiff_length_a            9.7985(3)
_cell_oxdiff_length_b            9.8928(3)
_cell_oxdiff_length_c            10.2589(4)
_cell_oxdiff_angle_alpha         94.490(3)
_cell_oxdiff_angle_beta          97.927(3)
_cell_oxdiff_angle_gamma         95.090(3)
_cell_oxdiff_volume              976.93(6)
_montpellier_reflns_maxres       0.66
_montpellier_reflns_completeness_maxres 93.94
_montpellier_reflns_redundancy_maxres 5.20
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV C(24,OCC) C(25,OCC) C(26,OCC)  C(27,OCC) C(28,OCC) 
CONT  H(241,OCC) H(242,OCC)  H(251,OCC) H(252,OCC) 
CONT  H(261,OCC) H(262,OCC)   H(271,OCC) H(272,OCC) 
CONT  H(281, OCC) H(282, OCC) 
CONT  C(29,OCC) C(30,OCC) C(31,OCC) C(32,OCC) C(33, OCC) 
CONT  H(291,OCC) H(292,OCC)  H(301,OCC) H(302,OCC)
CONT  H(311,OCC) H(312,OCC)   H(321,OCC) H(322,OCC) 
CONT  H(331, OCC) H(332, OCC) H(231,OCC) H(232,OCC) 
CONT H(233,OCC) H(234,OCC) 
WEIGHT -1  C(29,OCC) C(30,OCC) C(31,OCC) C(32,OCC) C(33, OCC) 
CONT  H(291,OCC) H(292,OCC)  H(301,OCC) H(302,OCC) 
CONT  H(311,OCC) H(312,OCC)   H(321,OCC) H(322,OCC) 
CONT  H(331, OCC) H(332, OCC) H(231,OCC) H(232,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   ( 171,X'S) H   ( 172,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 N   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S)  H   ( 223,X'S) 
RIDE C(  23,X'S) H( 231,X'S) H( 232,X'S) H( 233,X'S) H( 234,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S)
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE O(21,X'S) H(211,X'S) H(212,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = N(22) TO C(23) 
VIBR .0, 0.00200 = C(23) TO C(24) 
VIBR .0, 0.00200 = C(23) TO C(29) 
VIBR .0, 0.00500 = C(24) TO N(22)
VIBR .0, 0.00500 = C(29) TO N(22) 
VIBR .0, 0.00500 = C(29) TO C(24) 
VIBR .0, 0.00200 = C(24) TO C(25) 
VIBR .0, 0.00200 = C(24) TO C(30) 
VIBR .0, 0.00500 = C(25) TO C(23) 
VIBR .0, 0.00500 = C(30) TO C(23) 
VIBR .0, 0.00500 = C(30) TO C(25) 
VIBR .0, 0.00200 = C(25) TO C(26) 
VIBR .0, 0.00200 = C(25) TO C(29) 
VIBR .0, 0.00500 = C(26) TO C(24) 
VIBR .0, 0.00500 = C(29) TO C(24) 
VIBR .0, 0.00500 = C(29) TO C(26) 
VIBR .0, 0.00200 = C(26) TO C(27)
VIBR .0, 0.00200 = C(26) TO C(31) 
VIBR .0, 0.00200 = C(26) TO C(32) 
VIBR .0, 0.00500 = C(27) TO C(25) 
VIBR .0, 0.00500 = C(31) TO C(25) 
VIBR .0, 0.00500 = C(31) TO C(27)
VIBR .0, 0.00500 = C(32) TO C(25) 
VIBR .0, 0.00500 = C(32) TO C(27) 
VIBR .0, 0.00500 = C(32) TO C(31) 
VIBR .0, 0.00200 = C(27) TO C(28) 
VIBR .0, 0.00200 = C(27) TO C(31) 
VIBR .0, 0.00200 = C(27) TO C(33) 
VIBR .0, 0.00500 = C(28) TO C(26) 
VIBR .0, 0.00500 = C(31) TO C(26) 
VIBR .0, 0.00500 = C(31) TO C(28) 
VIBR .0, 0.00500 = C(33) TO C(26) 
VIBR .0, 0.00500 = C(33) TO C(28) 
VIBR .0, 0.00500 = C(33) TO C(31) 
VIBR .0, 0.00200 = C(28) TO C(28,-1,1,1,1) 
VIBR .0, 0.00200 = C(28) TO C(33,-1,1,1,1) 
VIBR .0, 0.00200 = C(28) TO C(32) 
VIBR .0, 0.00200 = C(28) TO C(33) 
VIBR .0, 0.00500 = C(28,-1,1,1,1) TO C(27) 
VIBR .0, 0.00500 = C(33,-1,1,1,1) TO C(27) 
VIBR .0, 0.00500 = C(33,-1,1,1,1) TO C(28,-1,1,1,1) 
VIBR .0, 0.00500 = C(32) TO C(27) 
VIBR .0, 0.00500 = C(32) TO C(28,-1,1,1,1) 
VIBR .0, 0.00500 = C(32) TO C(33,-1,1,1,1) 
VIBR .0, 0.00500 = C(33) TO C(27) 
VIBR .0, 0.00500 = C(33) TO C(28,-1,1,1,1) 
VIBR .0, 0.00500 = C(33) TO C(33,-1,1,1,1) 
VIBR .0, 0.00500 = C(33) TO C(32) 
VIBR .0, 0.00200 = C(29) TO C(30)
VIBR .0, 0.00500 = C(25) TO C(23)
VIBR .0, 0.00500 = C(30) TO C(23) 
VIBR .0, 0.00500 = C(30) TO C(25) 
VIBR .0, 0.00200 = C(30) TO C(31) 
VIBR .0, 0.00500 = C(24) TO C(29) 
VIBR .0, 0.00500 = C(31) TO C(29) 
VIBR .0, 0.00500 = C(31) TO C(24) 
VIBR .0, 0.00200 = C(31) TO C(32) 
VIBR .0, 0.00500 = C(26) TO C(30) 
VIBR .0, 0.00500 = C(27) TO C(30) 
VIBR .0, 0.00500 = C(27) TO C(26) 
VIBR .0, 0.00500 = C(32) TO C(30) 
VIBR .0, 0.00500 = C(32) TO C(26)
VIBR .0, 0.00500 = C(32) TO C(27)
VIBR .0, 0.00200 = C(32) TO C(33) 
VIBR .0, 0.00500 = C(28) TO C(31) 
VIBR .0, 0.00500 = C(26) TO C(31) 
VIBR .0, 0.00500 = C(26) TO C(28) 
VIBR .0, 0.00500 = C(33) TO C(31)
VIBR .0, 0.00500 = C(33) TO C(28) 
VIBR .0, 0.00500 = C(33) TO C(26) 
VIBR .0, 0.00200 = C(33) TO C(33,-1,1,1,1) 
VIBR .0, 0.00500 = C(27) TO C(32) 
VIBR .0, 0.00500 = C(33,-1,1,1,1) TO C(32) 
VIBR .0, 0.00500 = C(33,-1,1,1,1) TO C(27) 
VIBR .0, 0.00500 = C(28,-1,1,1,1) TO C(32) 
VIBR .0, 0.00500 = C(28,-1,1,1,1) TO C(27) 
VIBR .0, 0.00500 = C(28,-1,1,1,1) TO C(33,-1,1,1,1) 
VIBR .0, 0.00500 = C(28) TO C(32) 
VIBR .0, 0.00500 = C(28) TO C(27) 
VIBR .0, 0.00500 = C(28) TO C(33,-1,1,1,1) 
VIBR .0, 0.00500 = C(28) TO C(28,-1,1,1,1) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.08000 = N(22) TO C(23) 
U(IJ) .0, 0.04000 = C(23) TO C(24) 
U(IJ) .0, 0.04000 = C(23) TO C(29) 
U(IJ) .0, 0.04000 = C(24) TO C(25) 
U(IJ) .0, 0.04000 = C(24) TO C(30) 
U(IJ) .0, 0.04000 = C(25) TO C(26) 
U(IJ) .0, 0.04000 = C(25) TO C(29) 
U(IJ) .0, 0.04000 = C(26) TO C(27) 
U(IJ) .0, 0.04000 = C(26) TO C(31) 
U(IJ) .0, 0.04000 = C(26) TO C(32) 
U(IJ) .0, 0.04000 = C(27) TO C(28) 
U(IJ) .0, 0.04000 = C(27) TO C(31) 
U(IJ) .0, 0.04000 = C(27) TO C(33) 
U(IJ) .0, 0.04000 = C(28) TO C(28,-1,1,1,1) 
U(IJ) .0, 0.04000 = C(28) TO C(33,-1,1,1,1) 
U(IJ) .0, 0.04000 = C(28) TO C(32) 
U(IJ) .0, 0.04000 = C(28) TO C(33) 
U(IJ) .0, 0.04000 = C(29) TO C(30) 
U(IJ) .0, 0.04000 = C(30) TO C(31) 
U(IJ) .0, 0.04000 = C(31) TO C(32) 
U(IJ) .0, 0.04000 = C(32) TO C(33) 
U(IJ) .0, 0.04000 = C(33) TO C(33,-1,1,1,1) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;