A Clipped [3]Rotaxane Derived From Bis-nor-seco-Cucurbit[10]uril
James B. Wittenberg; Matthew G. Costales; Peter Y. Zavalij; Lyle Isaacs; Chem.Commun. 47 (2011) 9420–; doi:10.1039/c1cc13358f

data_7106775
_publ_section_title
;
 A Clipped [3]Rotaxane Derived From Bis-nor-seco-Cucurbit[10]uril
;
_journal_name_full               Chem.Commun.
_journal_page_first              9420
_journal_paper_doi               10.1039/c1cc13358f
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C68 H72 N44 O22, 2(C8 H14 N2), 18(H2 O), 4(I)'
_chemical_formula_sum            'C84 H136 I4 N48 O40'
_chemical_formula_weight         2966.01
_chemical_name_common            'CB10+ xylenediammonium diiodide hydrate'
_chemical_name_systematic
;
CB10+ bis-p-xylenediammonium diiodide octadecahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 93.1108(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.690(2)
_cell_length_b                   13.972(2)
_cell_length_c                   30.064(4)
_cell_measurement_reflns_used    15779
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.2
_cell_volume                     5742.1(14)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      610,610,310
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0533562
_diffrn_orient_matrix_UB_12      -0.0489077
_diffrn_orient_matrix_UB_13      -0.0004118
_diffrn_orient_matrix_UB_21      -0.0374951
_diffrn_orient_matrix_UB_22      0.0372221
_diffrn_orient_matrix_UB_23      -0.0236646
_diffrn_orient_matrix_UB_31      0.0331509
_diffrn_orient_matrix_UB_32      -0.0366711
_diffrn_orient_matrix_UB_33      -0.0234413
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            40898
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.99
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3016
_exptl_crystal_id                'Isaacs/Wittenberg JW-3-138 @250K'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.323
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         13130
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.260
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.01P)^2^+24.22P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                10224
_reflns_number_total             13130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc13358f.txt
_cod_data_source_block           1946
_cod_original_cell_volume        5742.3(15)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7106775
_diffrn_measurement_frame_width-ccd -0.30
_diffrn_measurement_total_frames-ccd 1330
_diffrn_measurement_frame_time-ccd 20
_diffrn_measurement_total_time-ccd 10
_diffrn_detector_distance-ccd    6.000
_diffrn_measurement_frame_size-ccd 512