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_7115928
_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
'C11 H28 N2, C16 H6 O12 S4, 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     other
_cell_angle_alpha                96.737(3)
_cell_angle_beta                 95.763(3)
_cell_angle_gamma                94.085(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8126(4)
_cell_length_b                   10.2605(4)
_cell_length_c                   19.4731(7)
_cell_measurement_reflns_used    5085
_cell_measurement_temperature    125
_cell_measurement_theta_max      28.6500
_cell_measurement_theta_min      2.0090
_cell_volume                     1930.37(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      125
_diffrn_detector_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_details
;
  1 omega  -24.00   58.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       17.7668 -100.0000 -180.0000 82

  2 omega  -51.00  -19.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       17.7668  -57.0000   30.0000 32

  3 omega  -54.00   43.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       17.7668  -38.0000  -90.0000 97

  4 omega   32.00   58.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       17.7668 -179.0000  -60.0000 26

  5 omega   -8.00   86.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       17.7668   77.0000   60.0000 94

  6 omega  -12.00   34.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       17.7668   77.0000  -60.0000 46

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0349949000
_diffrn_orient_matrix_UB_12      -0.0449600000
_diffrn_orient_matrix_UB_13      -0.0276864000
_diffrn_orient_matrix_UB_21      0.0589793000
_diffrn_orient_matrix_UB_22      -0.0360427000
_diffrn_orient_matrix_UB_23      -0.0011680000
_diffrn_orient_matrix_UB_31      -0.0248044000
_diffrn_orient_matrix_UB_32      -0.0394863000
_diffrn_orient_matrix_UB_33      0.0243776000
_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  0.022
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15112
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.969
_diffrn_reflns_theta_min         2.006
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97948
_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    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6676
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.0006551
_refine_ls_shift/su_mean         0.0000345
_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: 
 15.5 16.3 14.6 5.06 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0591
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0489
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                6676
_reflns_number_total             8700
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.06
_oxford_diffrn_Wilson_scale      0.07
_oxford_refine_ls_r_factor_ref   0.0418
_oxford_refine_ls_scale          2.549(4)
_oxford_reflns_number_all        8700
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c4cc03866e2.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_original_cell_volume        1930.36(13)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7115928
_cell_oxdiff_length_a            9.8099(4)
_cell_oxdiff_length_b            10.2612(4)
_cell_oxdiff_length_c            19.4704(7)
_cell_oxdiff_angle_alpha         96.760(3)
_cell_oxdiff_angle_beta          95.758(3)
_cell_oxdiff_angle_gamma         94.072(3)
_cell_oxdiff_volume              1929.65(13)
_montpellier_reflns_maxres       0.73
_montpellier_reflns_completeness_maxres 84.91
_montpellier_reflns_redundancy_maxres 1.74
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   6,X'S) H   (  36,X'S) 
RIDE C   (  15,X'S) H   (  33,X'S) 
RIDE C   (  16,X'S) H   (  11,X'S) 
RIDE C   (  23,X'S) H   (   1,X'S) 
RIDE C   (  24,X'S) H   (  25,X'S) 
RIDE C   (  28,X'S) H   (  13,X'S) 
RIDE O   (  33,X'S) H   (   3,X'S) H   (  55,X'S) 
RIDE O   (  34,X'S) H   (  48,X'S) H   (  50,X'S) 
RIDE N   (  35,X'S) H   (  20,X'S) H   (  24,X'S) H   (  43,X'S) 
RIDE C   (  36,X'S) H   (   6,X'S) H   (  10,X'S) 
RIDE C   (  37,X'S) H   (  37,X'S) H   (  38,X'S) 
RIDE C   (  38,X'S) H   (   5,X'S) H   (  15,X'S) 
RIDE C   (  39,X'S) H   (  26,X'S) H   (  39,X'S) 
RIDE C   (  40,X'S) H   (  18,X'S) H   (  27,X'S) 
RIDE C   (  41,X'S) H   (  28,X'S) H   (  44,X'S) 
RIDE C   (  42,X'S) H   (  23,X'S) H   (  30,X'S) 
RIDE C   (  43,X'S) H   (  14,X'S) H   (  34,X'S) 
RIDE C   (  44,X'S) H   (  41,X'S) H   (  49,X'S) 
RIDE N   (  45,X'S) H   (   2,X'S) H   (  19,X'S) 
RIDE N   (  47,X'S) H   (   7,X'S) H   (   9,X'S) 
RIDE N   (  48,X'S) H   (  16,X'S) H   (  21,X'S) 
RIDE N   (  49,X'S) H   (   4,X'S) H   (  31,X'S)
RIDE N   (  51,X'S) H   (  29,X'S) H   (  45,X'S) 
RIDE N   (  52,X'S) H   (   8,X'S) H   (  35,X'S) 
RIDE N   (  53,X'S) H   (  12,X'S) H   (  22,X'S) H   (  47,X'S) 
RIDE C   (  54,X'S) H   (  17,X'S) H   (  32,X'S) 
RIDE C   (   1,X'S) H   (  40,X'S) H   (  46,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                                                                             
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