Constructions of two polycatenanes and one polypseudo-rotaxane by discrete tetrahedral cages and stool-like building units
Long Jiang; Ping Ju; Xian-Rui Meng; Xiao-Jun Kuang; Tong-Bu Lu; Scientific Reports 2 (2012) 668–; doi:10.1038/srep00668

data_1548642
_publ_section_title
;
 Constructions of two polycatenanes and one polypseudo-rotaxane by
 discrete tetrahedral cages and stool-like building units
;
_journal_name_full               'Scientific Reports'
_journal_page_first              668
_journal_paper_doi               10.1038/srep00668
_journal_volume                  2
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         '4(C31 H39 N5 Ni O6), 37(H2 O)'
_chemical_formula_sum            'C124 H230 N20 Ni4 O61'
_chemical_formula_weight         3212.02
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   30.0315(4)
_cell_length_b                   30.0315(4)
_cell_length_c                   8.8752(2)
_cell_measurement_reflns_used    10099
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      66.8985
_cell_measurement_theta_min      2.9405
_cell_volume                     8004.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 10.5058
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -89.00  -64.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7938  136.0000  141.0000 25

  2 omega  -35.00   66.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7938  -38.0000 -120.0000 101

  3 omega -120.00  -89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  136.0000  -38.0000 31

  4 omega   61.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -91.0000 -142.0000 50

  5 omega   45.00   71.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -90.0000 26

  6 omega   82.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000 -150.0000 31

  7 omega   86.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -180.0000 26

  8 omega   63.00  117.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  120.0000 54

  9 omega  126.00  152.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  120.0000 26

 10 omega  133.00  168.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000 -150.0000 35

 11 omega   52.00   77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -22.0000  160.0000 25

 12 omega   40.00   77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   30.0000 37

 13 omega  116.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000 -150.0000 58

 14 omega   68.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -89.0000 -115.0000 41

 15 omega  143.00  168.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000  -90.0000 25

 16 omega   12.00   37.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -89.0000 -115.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0163330000
_diffrn_orient_matrix_UB_12      -0.0485615000
_diffrn_orient_matrix_UB_13      0.0062281000
_diffrn_orient_matrix_UB_21      0.0486482000
_diffrn_orient_matrix_UB_22      0.0163372000
_diffrn_orient_matrix_UB_23      -0.0028368000
_diffrn_orient_matrix_UB_31      0.0001872000
_diffrn_orient_matrix_UB_32      0.0020692000
_diffrn_orient_matrix_UB_33      0.1734686000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            15842
_diffrn_reflns_theta_full        67.01
_diffrn_reflns_theta_max         67.01
_diffrn_reflns_theta_min         4.66
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3418
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         6579
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0655
_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^)+(0.1429P)^2^+4.6770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.1744
_reflns_number_gt                6524
_reflns_number_total             6579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Sci-Rep-2012-2-668-1.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C124 H230 N20 O61 Ni4'
_cod_database_code               1548642