Linking [2]rotaxane wheels to create a new type of metal organic rotaxane framework
Stephen Loeb; Darren Mercer; Nicholas Vukotic; Chem.Commun. 47 (2011) 896–; doi:10.1039/c0cc04139d

data_7105867
_publ_section_title
;
 Linking [2]rotaxane wheels to create a new type of metal organic rotaxane
 framework
;
_journal_name_full               Chem.Commun.
_journal_page_first              896
_journal_paper_doi               10.1039/c0cc04139d
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C104 H134 B2 Cd2 Cl4 F8 N14 O36'
_chemical_formula_weight         2696.47
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.151(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.006(2)
_cell_length_b                   18.712(2)
_cell_length_c                   19.944(3)
_cell_measurement_temperature    173(2)
_cell_volume                     6204.3(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_molecular_graphics    'Bruker SHELXTL XP'
_computing_publication_material  'Bruker SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38654
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.5633
_exptl_absorpt_correction_T_min  0.5013
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             2780
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
The unit cell contains 16 molecules of nitromethane which have been
treated as a diffuse contribution to the overall scattering without
specific atom positions by SQUEEZE/PLATON.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The non-coordinating chloride anion is disordered over three positions
which were modelled as 45%, 45% and 10% occupancy and restrained with SIMU
to have comparable thermal parameters. There was also evidence of disorder
at the (H2O)2Cd(mu-Cl)2Cd(H2O)2 core, but this could not be modelled
satisfactorily. As a result, the final structure displays elongated
thermal parameters for these atoms.
;
_refine_diff_density_max         1.912
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.537
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         6488
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.544
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.1195
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3443
_refine_ls_wR_factor_ref         0.3638
_reflns_number_gt                4890
_reflns_number_total             6488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC04139D.TXT
_cod_data_source_block           dm72
_cod_original_cell_volume        6204.2(14)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7105867