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_7115926
_publ_section_title
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 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, 2(C10 H26 N2), 4(H2 O)'
_chemical_formula_sum            'C36 H66 N4 O16 S4'
_chemical_formula_weight         939.21
_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                77.311(3)
_cell_angle_beta                 81.835(4)
_cell_angle_gamma                86.214(3)
_cell_formula_units_Z            1
_cell_length_a                   7.8956(4)
_cell_length_b                   9.6557(3)
_cell_length_c                   14.9160(6)
_cell_measurement_reflns_used    6458
_cell_measurement_temperature    175
_cell_measurement_theta_max      29.0590
_cell_measurement_theta_min      2.3010
_cell_volume                     1097.43(8)
_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 1.000
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_details
;
  1 omega  -53.00   44.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -       15.4892  -19.0000  -90.0000 97

  2 omega   49.00   88.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -       15.4892  179.0000 -150.0000 39

  3 omega  -52.00   15.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -       15.4892  -57.0000   30.0000 67

  4 omega  -82.00   -5.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.2704  -57.0000 -120.0000 77

  5 omega  -86.00  -51.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.2704  151.0000  -49.2221 35

  6 omega  -47.00    8.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.2704  -77.0000  150.0000 55

  7 omega   34.00   88.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -       15.4892  179.0000  -60.0000 54

  8 omega  -33.00   51.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.2704   57.0000  150.0000 84

  9 omega  -85.00    3.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.2704  -38.0000   60.0000 88

 10 omega  -84.00  -59.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.2704  -57.0000    0.0000 25

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0824545000
_diffrn_orient_matrix_UB_12      0.0249365000
_diffrn_orient_matrix_UB_13      0.0001357000
_diffrn_orient_matrix_UB_21      0.0322593000
_diffrn_orient_matrix_UB_22      -0.0314879000
_diffrn_orient_matrix_UB_23      -0.0380024000
_diffrn_orient_matrix_UB_31      -0.0201907000
_diffrn_orient_matrix_UB_32      0.0637491000
_diffrn_orient_matrix_UB_33      -0.0311959000
_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  0.032
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15468
_diffrn_reflns_theta_full        26.370
_diffrn_reflns_theta_max         29.386
_diffrn_reflns_theta_min         2.163
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97075
_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    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             502
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0944
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4495
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.0014653
_refine_ls_shift/su_mean         0.0000751
_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: 
 9.17 2.69 7.17 1.57 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0532
_refine_ls_wR_factor_gt          0.0483
_refine_ls_wR_factor_ref         0.0483
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              13
_reflns_limit_k_min              -12
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                4495
_reflns_number_total             5259
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.72
_oxford_diffrn_Wilson_scale      0.42
_oxford_refine_ls_r_factor_ref   0.0437
_oxford_refine_ls_scale          4.558(8)
_oxford_reflns_number_all        5259
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c4cc03866e2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7115926
_cell_oxdiff_length_a            7.8956(4)
_cell_oxdiff_length_b            9.6557(3)
_cell_oxdiff_length_c            14.9160(6)
_cell_oxdiff_angle_alpha         77.311(3)
_cell_oxdiff_angle_beta          81.835(4)
_cell_oxdiff_angle_gamma         86.214(3)
_cell_oxdiff_volume              1097.43(8)
_montpellier_reflns_maxres       0.72
_montpellier_reflns_completeness_maxres 86.85
_montpellier_reflns_redundancy_maxres 2.94
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'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   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = C(26) TO C(271) 
VIBR .0, 0.00500 = C(271) TO C(25) 
VIBR .0, 0.00200 = N(30) TO C(290) 
VIBR .0, 0.00200 = N(30) TO C(291) 
VIBR .0, 0.00500 = C(291) TO C(290) 
VIBR .0, 0.00200 = C(280) TO C(281) 
VIBR .0, 0.00200 = C(280) TO C(290) 
VIBR .0, 0.00200 = C(280) TO C(291) 
VIBR .0, 0.00200 = C(280) TO C(271) 
VIBR .0, 0.00500 = C(290) TO C(281) 
VIBR .0, 0.00500 = C(291) TO C(281)
VIBR .0, 0.00500 = C(291) TO C(290) 
VIBR .0, 0.00500 = C(271) TO C(281) 
VIBR .0, 0.00500 = C(271) TO C(290) 
VIBR .0, 0.00500 = C(271) TO C(291) 
VIBR .0, 0.00200 = C(281) TO C(290) 
VIBR .0, 0.00200 = C(281) TO C(291) 
VIBR .0, 0.00200 = C(281) TO C(271) 
VIBR .0, 0.00500 = C(290) TO C(280) 
VIBR .0, 0.00500 = C(291) TO C(280) 
VIBR .0, 0.00500 = C(291) TO C(290) 
VIBR .0, 0.00500 = C(271) TO C(280) 
VIBR .0, 0.00500 = C(271) TO C(290) 
VIBR .0, 0.00500 = C(271) TO C(291) 
VIBR .0, 0.00200 = C(290) TO C(291) 
VIBR .0, 0.00500 = C(281) TO N(30)
VIBR .0, 0.00500 = C(280) TO N(30) 
VIBR .0, 0.00500 = C(280) TO C(281) 
VIBR .0, 0.00500 = C(291) TO N(30) 
VIBR .0, 0.00500 = C(291) TO C(281) 
VIBR .0, 0.00500 = C(291) TO C(280) 
VIBR .0, 0.00500 = C(280) TO N(30) 
VIBR .0, 0.00500 = C(281) TO N(30) 
VIBR .0, 0.00500 = C(281) TO C(280) 
VIBR .0, 0.00500 = C(290) TO N(30) 
VIBR .0, 0.00500 = C(290) TO C(280) 
VIBR .0, 0.00500 = C(290) TO C(281) 
VIBR .0, 0.00500 = C(280) TO C(26) 
VIBR .0, 0.00500 = C(281) TO C(26) 
VIBR .0, 0.00500 = C(281) TO C(280) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(26) TO C(271) 
U(IJ) .0, 0.04000 = N(30) TO C(290) 
U(IJ) .0, 0.04000 = N(30) TO C(291) 
U(IJ) .0, 0.04000 = C(280) TO C(281) 
U(IJ) .0, 0.04000 = C(280) TO C(290) 
U(IJ) .0, 0.04000 = C(280) TO C(291) 
U(IJ) .0, 0.04000 = C(280) TO C(271) 
U(IJ) .0, 0.04000 = C(281) TO C(290) 
U(IJ) .0, 0.04000 = C(281) TO C(291) 
U(IJ) .0, 0.04000 = C(281) TO C(271) 
U(IJ) .0, 0.04000 = C(290) TO C(291) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;