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_7115929
_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
'C16 H6 O12 S4, C11 H28 N2, 2(C H6 N3), 2(H2 O)'
_chemical_formula_sum            'C29 H50 N8 O14 S4'
_chemical_formula_weight         863.05
_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                96.289(3)
_cell_angle_beta                 95.622(3)
_cell_angle_gamma                94.839(3)
_cell_formula_units_Z            1
_cell_length_a                   9.8826(4)
_cell_length_b                   10.2939(4)
_cell_length_c                   9.8156(4)
_cell_measurement_reflns_used    8267
_cell_measurement_temperature    293
_cell_measurement_theta_max      32.0910
_cell_measurement_theta_min      2.0830
_cell_volume                     983.19(7)
_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      293
_diffrn_detector_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_details
;
  1 omega   12.00   72.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   19.0000  150.0000 60

  2 omega   68.00   95.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   57.0000 -150.0000 27

  3 omega  -23.00   68.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169 -100.0000   60.0000 91

  4 omega   28.00   96.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   77.0000  -60.0000 68

  5 omega   43.00   68.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169 -100.0000 -180.0000 25

  6 omega   10.00   93.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   57.0000 -180.0000 83

  7 omega   -1.00   68.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169 -100.0000  -90.0000 69

  8 omega -103.00  -78.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.9544  179.0000 -150.0000 25

  9 omega   -4.00   96.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   77.0000  150.0000 100

 10 omega    5.00   95.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   57.0000  -90.0000 90

 11 omega  -43.00   46.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169  -57.0000 -180.0000 89

 12 omega   34.00  102.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169  179.0000   60.0000 68

 13 omega -103.00  -56.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.9544 -179.0000    0.0000 47

 14 omega  -97.00    3.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.9544  -77.0000   30.0000 100

 15 omega   -4.00   96.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   77.0000  -30.0000 100

 16 omega   34.00  102.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169  179.0000  150.0000 68

 17 omega   34.00   84.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169  179.0000    0.0000 50

 18 omega  -43.00   46.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169  -57.0000  120.0000 89

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0581866000
_diffrn_orient_matrix_UB_12      0.0257566000
_diffrn_orient_matrix_UB_13      0.0243784000
_diffrn_orient_matrix_UB_21      0.0219316000
_diffrn_orient_matrix_UB_22      0.0657031000
_diffrn_orient_matrix_UB_23      -0.0178313000
_diffrn_orient_matrix_UB_31      -0.0384888000
_diffrn_orient_matrix_UB_32      -0.0164025000
_diffrn_orient_matrix_UB_33      -0.0627459000
_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     0.0473
_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       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31497
_diffrn_reflns_theta_full        28.552
_diffrn_reflns_theta_max         32.446
_diffrn_reflns_theta_min         2.000
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98185
_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            colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0233
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5199
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.0004576
_refine_ls_shift/su_mean         0.0000217
_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 14.1 13.5 4.57 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0632
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0539
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                5199
_reflns_number_total             6688
_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   0.0479
_oxford_refine_ls_scale          4.238(9)
_oxford_reflns_number_all        6688
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c4cc03866e2.cif
_cod_data_source_block           1c
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7115929
_cell_oxdiff_length_a            9.8156(4)
_cell_oxdiff_length_b            9.8831(4)
_cell_oxdiff_length_c            10.2952(4)
_cell_oxdiff_angle_alpha         94.845(3)
_cell_oxdiff_angle_beta          96.293(3)
_cell_oxdiff_angle_gamma         95.622(3)
_cell_oxdiff_volume              983.34(7)
_montpellier_reflns_maxres       0.66
_montpellier_reflns_completeness_maxres 94.29
_montpellier_reflns_redundancy_maxres 4.71
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE N   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE N   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE N   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE N   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S)  H   ( 183,X'S) 
RIDE C   (  191,X'S) H   ( 1911,X'S) H   ( 1912,X'S) 
RIDE C   (  201,X'S) H   ( 2011,X'S) H   ( 2012,X'S) 
RIDE C   (  211,X'S) H   ( 2111,X'S) H   ( 2112,X'S) 
RIDE C   (  221,X'S) H   ( 2211,X'S) H   ( 2212,X'S) 
RIDE C   (  192,X'S) H   ( 1921,X'S) H   ( 1922,X'S)
RIDE C   (  202,X'S) H   ( 2021,X'S) H   ( 2022,X'S) 
RIDE C   (  212,X'S) H   ( 2121,X'S) H   ( 2122,X'S)
RIDE C   (  222,X'S) H   ( 2221,X'S) H   ( 2222,X'S) 
RIDE C   (  232,X'S) H   ( 2321,X'S) H   ( 2322,X'S) 
RIDE C   (  241,X'S) H   ( 2411,X'S) H   ( 2412,X'S) 
RIDE C   (  242,X'S) H   ( 2421,X'S) H   ( 2422,X'S) 
RIDE O(17,X'S) H(171,X'S) H(172,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.02 = C(191) TO C(192), C(201) TO C(202), C(211) TO C(212), 
CONT C(221) TO C(222), C(241) TO C(242), C(232) TO C(241), C(232) TO C(222) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;