In silico Design of Supramolecules from Their Precursors: Odd-Even Effects in Cage-Forming Reactions
Kim E. Jelfs; Edward G. B. Eden; Jamie L. Culshaw; Stephen Shakespeare; Edward O. Pyzer-Knapp; Hugh P. G. Thompson; John Bacsa; Graeme M. Day; Dave J. Adams; Andrew I. Cooper; Journal of the American Chemical Society 135 (2013) 9307–9310; doi:10.1021/ja404253j

data_4119994
_publ_contact_author_name
;
;
_publ_section_title
;
 In silico Design of Supramolecules from Their Precursors: Odd-Even
 Effects in Cage-Forming Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9307
_journal_page_last               9310
_journal_paper_doi               10.1021/ja404253j
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         '(C66 H84 N12).7(C H4 O)'
_chemical_formula_sum            'C73 H112 N12 O7'
_chemical_formula_weight         1269.75
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-21
_audit_creation_method
;
  Olex2 1.2-alpha
  (compiled Mar 30 2012 14:36:40, GUI svn.r4156)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 116.661(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.251(3)
_cell_length_b                   8.8610(10)
_cell_length_c                   26.926(2)
_cell_measurement_reflns_used    269
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.45
_cell_measurement_theta_min      2.37
_cell_volume                     7516.3(12)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 v2011.2-4 (Bruker, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker D8 diffractometer with APEX detector'
_diffrn_measurement_method       '\w scans with a narrow frame width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0774
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            16746
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.29
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0891 before and 0.0476 after correction.
The Ratio of minimum to maximum transmission is 0.8309.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       needle
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 Squeeze calculates 8 solvent accessible voids per unit cell  
 and 128 electrons for each formula unit, corresponding to 
 an additional 7 methanol molecules for each molecular formula unit
 or 6 methanol molecules and 2 water molecules. 

;
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1474
_refine_ls_R_factor_gt           0.0998
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+26.9369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2020
_refine_ls_wR_factor_ref         0.2197
_reflns_number_gt                4235
_reflns_number_total             6779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404253j_si_002.cif
_cod_data_source_block           ss27070m
_cod_database_code               4119994