Photocontrol over Cucurbit[8]uril Complexes: Stoichiometry and Supramolecular Polymers
Jesús del Barrio; Peter N. Horton; Didier Lairez; Gareth O. Lloyd; Chris Toprakcioglu; Oren A. Scherman; Journal of the American Chemical Society 135 (2013) 11760–11763; doi:10.1021/ja406556h

data_4120293
_publ_section_title
;
 Photocontrol over Cucurbit[8]uril Complexes: Stoichiometry and
 Supramolecular Polymers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11760
_journal_page_last               11763
_journal_paper_doi               10.1021/ja406556h
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C72 H81 Cl0.5 I1.5 N36 O21.5'
_chemical_formula_weight         2002.80
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9176(9)
_cell_length_b                   26.8483(19)
_cell_length_c                   25.9955(18)
_cell_measurement_reflns_used    13801
_cell_measurement_temperature    30(2)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      1.1
_cell_volume                     9015.6(11)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2012)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      30(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            67900
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         24.207
_diffrn_reflns_theta_min         2.841
_diffrn_source                   synchrotron
_diffrn_source_type              'DLS beamline I19'
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       plate
_exptl_crystal_F_000             4100
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.158
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.52(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1333
_refine_ls_number_reflns         15777
_refine_ls_number_restraints     2475
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1527
_refine_ls_R_factor_gt           0.1030
_refine_ls_shift/su_max          0.083
_refine_ls_shift/su_mean         0.005
_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          0.2845
_refine_ls_wR_factor_ref         0.3268
_reflns_Friedel_coverage         0.955
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                9635
_reflns_number_total             15777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja406556h_si_003.cif
_cod_data_source_block           shelxl
_cod_original_formula_sum        'C72 H81 Cl0.50 I1.50 N36 O21.50'
_cod_database_code               4120293
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2013-3
_shelx_res_checksum              51080