Rotaxanes from Tetralactams
Gibson, Harry W.; Wang, Hong; Niu, Zhenbin; Slebodnick, Carla; Zhakharov, Lev N.; Rheingold, Arnold L.; Macromolecules 45 (2012) 1270–; doi:10.1021/ma202373x

data_1503456
_publ_section_title
;
 Rotaxanes from Tetralactams
;
_journal_issue                   3
_journal_name_full               Macromolecules
_journal_page_first              1270
_journal_paper_doi               10.1021/ma202373x
_journal_volume                  45
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C82 H94 O2, C67 H70 N4 O5, 2(C3 H6 O)'
_chemical_formula_sum            'C155 H176 N4 O9'
_chemical_formula_weight         2239.00
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_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                75.588(6)
_cell_angle_beta                 87.355(6)
_cell_angle_gamma                77.305(7)
_cell_formula_units_Z            1
_cell_length_a                   11.6351(9)
_cell_length_b                   16.2914(12)
_cell_length_c                   20.4165(13)
_cell_measurement_reflns_used    6474
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.7079
_cell_measurement_theta_min      3.8905
_cell_volume                     3656.4(5)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_publication_material
'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_structure_refinement
'SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_structure_solution
'SHELXS-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 16.0122
_diffrn_detector_type            'Oxford Diffraction Eos'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      -0.0887485494
_diffrn_orient_matrix_UB_12      -0.0586208004
_diffrn_orient_matrix_UB_13      0.0211528992
_diffrn_orient_matrix_UB_21      -0.0343894527
_diffrn_orient_matrix_UB_22      0.0382694251
_diffrn_orient_matrix_UB_23      0.0613192462
_diffrn_orient_matrix_UB_31      -0.0958799478
_diffrn_orient_matrix_UB_32      0.0709190839
_diffrn_orient_matrix_UB_33      -0.0425282399
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_sigmaI/netI    0.1569
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46147
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         70.69
_diffrn_reflns_theta_min         3.89
_diffrn_source                   'Nova (Cu) X-ray Source'
_diffrn_source_current           1
_diffrn_source_voltage           50
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.51 (release 27-10-2009 CrysAlis171 .NET)
 (compiled Oct 27 2009,12:04:35)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1206
_exptl_crystal_size_max          0.114
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.828
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         13558
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      0.826
_refine_ls_R_factor_all          0.1877
_refine_ls_R_factor_gt           0.1011
_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^)+(0.1806P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2651
_refine_ls_wR_factor_ref         0.3075
_reflns_number_gt                4671
_reflns_number_total             13558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ma202373x_si_002.cif
_cod_data_source_block           cs1445
_cod_database_code               1503456