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_7115927
_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, C10 H26 N2, 2(C H6 N3), 2(H2 O)'
_chemical_formula_sum            'C28 H48 N8 O14 S4'
_chemical_formula_weight         849.02
_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                95.207(6)
_cell_angle_beta                 95.926(6)
_cell_angle_gamma                95.224(7)
_cell_formula_units_Z            1
_cell_length_a                   9.7336(8)
_cell_length_b                   9.7556(8)
_cell_length_c                   10.1940(7)
_cell_measurement_reflns_used    6774
_cell_measurement_temperature    175
_cell_measurement_theta_max      32.3830
_cell_measurement_theta_min      2.1090
_cell_volume                     953.91(13)
_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 1.000
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
  1 omega  -24.00   67.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732 -100.0000  150.0000 91

  2 omega   35.00   92.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732  179.0000  150.0000 57

  3 omega    4.00   99.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732   38.0000  -60.0000 95

  4 omega   -4.00   96.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732   77.0000   90.0000 100

  5 omega    5.00   95.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732   57.0000 -150.0000 90

  6 omega    5.00   95.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732   57.0000   30.0000 90

  7 omega   34.00  102.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732  179.0000   90.0000 68

  8 omega   34.00  102.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732  179.0000  -30.0000 68

  9 omega -103.00  -56.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -      -26.9544 -179.0000 -180.0000 47

 10 omega  -24.00   69.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732 -100.0000  -30.0000 93

 11 omega    0.00   95.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732   71.0000  -72.0000 95

 12 omega  -52.00  -27.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -      -26.9544   38.0000 -120.0000 25

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0164071000
_diffrn_orient_matrix_UB_12      0.0404693000
_diffrn_orient_matrix_UB_13      0.0565565000
_diffrn_orient_matrix_UB_21      0.0073328000
_diffrn_orient_matrix_UB_22      0.0600098000
_diffrn_orient_matrix_UB_23      -0.0338628000
_diffrn_orient_matrix_UB_31      -0.0711515000
_diffrn_orient_matrix_UB_32      -0.0113477000
_diffrn_orient_matrix_UB_33      -0.0241764000
_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     0.0408
_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       -15
_diffrn_reflns_number            36619
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         32.489
_diffrn_reflns_theta_min         2.019
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98990
_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    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.48
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5743
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.0008218
_refine_ls_shift/su_mean         0.0000709
_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: 
 0.584 -10.0 -3.38 -3.86 -2.49 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0343
_refine_ls_wR_factor_gt          0.0299
_refine_ls_wR_factor_ref         0.0299
_reflns_limit_h_max              14
_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                5743
_reflns_number_total             6564
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.57
_oxford_diffrn_Wilson_scale      0.32
_oxford_refine_ls_r_factor_ref   0.0353
_oxford_refine_ls_scale          5.076(4)
_oxford_reflns_number_all        6564
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c4cc03866e2.cif
_cod_data_source_block           1a
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7115927
_cell_oxdiff_length_a            9.7662(4)
_cell_oxdiff_length_b            9.7818(5)
_cell_oxdiff_length_c            10.2045(5)
_cell_oxdiff_angle_alpha         95.342(4)
_cell_oxdiff_angle_beta          95.497(4)
_cell_oxdiff_angle_gamma         95.663(4)
_cell_oxdiff_volume              960.43(8)
_montpellier_reflns_maxres       0.66
_montpellier_reflns_completeness_maxres 93.05
_montpellier_reflns_redundancy_maxres 3.50
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (  10,X'S) H   (   3,X'S) 
RIDE C   (  15,X'S) H   (  14,X'S) 
RIDE C   (  16,X'S) H   (   2,X'S) 
RIDE O   (  17,X'S) H   (  21,X'S) H   (  24,X'S) 
RIDE N   (  18,X'S) H   (   6,X'S) H   (   7,X'S) 
RIDE N   (  20,X'S) H   (   8,X'S) H   (  13,X'S) 
RIDE N   (  21,X'S) H   (  15,X'S) H   (  26,X'S) 
RIDE N   (  22,X'S) H   (   1,X'S) H   (   5,X'S) H   (  10,X'S) 
RIDE C   (  23,X'S) H   (  16,X'S) H   (  18,X'S)
RIDE C   (  24,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (  25,X'S) H   (  20,X'S) H   (  22,X'S) 
RIDE C   (  26,X'S) H   (   9,X'S) H   (  17,X'S) 
RIDE C   (  27,X'S) H   (   4,X'S) H   (  19,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) 
END                                                                             
;