Solvent and hydrogen confinement in molecular capsules – Hirshfeld surface and molecular simulation analysis
Martin, Adam D.; Boulos, Ramiz A.; Iyer, K. Swaminathan; Sobolev, Alexandre N.; Bond, Charles S.; Atwood, Jerry L.; Dalgarno, Scott J.; Raston, Colin L.; Chemical Communications (Cambridge, United Kingdom) 47 (2011) 9882–9884; doi:10.1039/c1cc13038b

data_7106794
_publ_section_title
;
 Solvent and hydrogen confinement in molecular capsules -- Hirshfeld surface and
 molecular simulation analysis
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   35
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              9882
_journal_page_last               9884
_journal_paper_doi               10.1039/c1cc13038b
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety
'3(C44 H56 O12), 2(C4 H8 O2), 4(C H Cl3), 7(H2 O)'
_chemical_formula_sum            'C144 H202 Cl12 O47'
_chemical_formula_weight         3110.46
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                117.451(1)
_cell_angle_beta                 92.363(4)
_cell_angle_gamma                118.837(2)
_cell_formula_units_Z            2
_cell_length_a                   22.1023(5)
_cell_length_b                   22.4800(5)
_cell_length_c                   22.6463(18)
_cell_measurement_reflns_used    27708
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      51.7
_cell_measurement_theta_min      2.4
_cell_volume                     8228.8(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_molecular_graphics    'X-Seed 2.0 (Barbour, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra, Ruby CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            73260
_diffrn_reflns_theta_full        51.76
_diffrn_reflns_theta_max         51.76
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    2.485
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3292
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.596
_refine_diff_density_min         -1.738
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1809
_refine_ls_number_reflns         17852
_refine_ls_number_restraints     561
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1939
_refine_ls_R_factor_gt           0.1535
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+150.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3441
_refine_ls_wR_factor_ref         0.3634
_reflns_number_gt                11728
_reflns_number_total             17852
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc13038b.txt
_cod_data_source_block           cb081004
_cod_original_cell_volume        8228.8(7)
_cod_database_code               7106794