Encapsulation and solid state sequestration of gases by calix[6]arene-based molecular containers
Lavendomme, Roy; Ajami, Daniela; Moerkerke, Steven; Wouters, Johan; Rissanen, Kari; Luhmer, Michel; Jabin, Ivan; Chem. Commun.  (2017) –; doi:10.1039/C7CC03078A

data_7120172
_publ_section_title
;
 Encapsulation and solid state sequestration of gases by
 calix[6]arene-based molecular containers
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03078A
_journal_year                    2017
_chemical_formula_moiety         '4(C2H4Cl2), C96H144N6O12'
_chemical_formula_sum            'C104 H138 Cl8 N6 O12'
_chemical_formula_weight         1947.8
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-06
_audit_creation_method           SHELXL-2014/8
_audit_update_record
;
2017-04-18 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                97.571(4)
_cell_angle_beta                 109.693(5)
_cell_angle_gamma                114.255(5)
_cell_formula_units_Z            1
_cell_length_a                   13.7784(9)
_cell_length_b                   14.3195(7)
_cell_length_c                   16.9560(8)
_cell_measurement_reflns_used    3116
_cell_measurement_temperature    149.8
_cell_measurement_theta_max      62.3786
_cell_measurement_theta_min      3.5638
_cell_volume                     2725.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.8
_diffrn_detector_area_resol_mean 5.1856
_diffrn_measured_fraction_theta_full 0.855
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_details
;
  1 omega  -28.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -1.1041   38.0000    0.0000 103

  2 omega -117.00  -13.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   77.0000   30.0000 104

  3 omega -171.00    5.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000    0.0000    0.0000 176

  4 omega   10.00  114.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       83.9257  -61.0000  120.0000 104

  5 omega   18.00   97.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       83.9257 -126.0000  120.0000 79
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0113631000
_diffrn_orient_matrix_UB_12      -0.0468253000
_diffrn_orient_matrix_UB_13      0.0773391000
_diffrn_orient_matrix_UB_21      0.0932832000
_diffrn_orient_matrix_UB_22      0.1136652000
_diffrn_orient_matrix_UB_23      0.0652387000
_diffrn_orient_matrix_UB_31      -0.0983582000
_diffrn_orient_matrix_UB_32      0.0185291000
_diffrn_orient_matrix_UB_33      0.0099567000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.855
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9569
_diffrn_reflns_point_group_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        62.470
_diffrn_reflns_theta_max         62.470
_diffrn_reflns_theta_min         3.567
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.35
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.523
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.649
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         7431
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.611
_refine_ls_R_factor_all          0.1620
_refine_ls_R_factor_gt           0.1316
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3837
_refine_ls_wR_factor_ref         0.4171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5252
_reflns_number_total             7431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc03078a2.cif
_cod_data_source_block           C2H4Cl2_4
_cod_database_code               7120172
_shelx_shelxl_version_number     2016/4
_reflns_odcompleteness_completeness 90.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_shelx_res_checksum              95353
_shelx_hkl_checksum              48222