Synthesis, Structure, and Dynamic Properties of Hybrid Organic-Inorganic Rotaxanes
Beatriz Ballesteros; Thomas B. Faust; Chin-Fa Lee; David A. Leigh; Christopher A. Muryn; Robin G. Pritchard; David Schultz; Simon J. Teat; Grigore A. Timco; Richard E. P. Winpenny; Journal of the American Chemical Society 132 (2010) 15435–15444; doi:10.1021/ja1074773

data_4103428
_publ_section_title
;
 Synthesis, Structure, and Dynamic Properties of Hybrid Organic-Inorganic
 Rotaxanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15435
_journal_page_last               15444
_journal_paper_doi               10.1021/ja1074773
_journal_volume                  132
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
;
4(C80 H144 Cd Cr7 F8 O32), 4(C22 H46 N3 O2), 6(C3 H6 O), 2(O)
;
_chemical_formula_sum            'C106.5 H199 Cd Cr7 F8 N3 O36'
_chemical_formula_weight         2726.09
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-06-17T13:59:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.7900(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8642(2)
_cell_length_b                   32.2599(4)
_cell_length_c                   28.2099(5)
_cell_measurement_reflns_used    19016
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.722
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     15313.7(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.551801E-1
_diffrn_orient_matrix_UB_12      0.112483E-1
_diffrn_orient_matrix_UB_13      -0.6004E-3
_diffrn_orient_matrix_UB_21      0.124112E-1
_diffrn_orient_matrix_UB_22      -0.104114E-1
_diffrn_orient_matrix_UB_23      0.330486E-1
_diffrn_orient_matrix_UB_31      0.182404E-1
_diffrn_orient_matrix_UB_32      -0.269438E-1
_diffrn_orient_matrix_UB_33      -0.130209E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.1014
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24887
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        20
_diffrn_reflns_theta_max         20
_diffrn_reflns_theta_min         2.91
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2008/1 (Bruker,2008) was used for absorption correction.
 R(int) was 0.0626 before and 0.0395 after correction.
 The Ratio of minimum to maximum transmission is 0.823734261988.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5740
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1441
_refine_ls_number_reflns         14203
_refine_ls_number_restraints     2481
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+80.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2391
_reflns_number_gt                8588
_reflns_number_total             14203
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja1074773_si_013.cif
_cod_data_source_block           ROB
_cod_original_formula_sum        'C106.50 H199 Cd Cr7 F8 N3 O36'
_cod_database_code               4103428