Coordination-Driven Polymerization of Supramolecular Nanocages.
Niu, Zheng; Fang, Sheng; Liu, Xiao; Ma, Jian-Gong; Ma, Shengqian; Cheng, Peng; Journal of the American Chemical Society 137 (2015) 14873–14876; doi:10.1021/jacs.5b10815

data_4129840
_publ_section_title
;
 Coordination-Driven Polymerization of Supramolecular Nanocages.
;
_journal_issue                   47
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14873
_journal_page_last               14876
_journal_paper_doi               10.1021/jacs.5b10815
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C281 H434 Cu24 O212 S10'
_chemical_formula_sum            'C281 H434 Cu24 O212 S10'
_chemical_formula_weight         9050.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-12-20
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                61.777(2)
_cell_angle_beta                 63.599(3)
_cell_angle_gamma                77.407(2)
_cell_formula_units_Z            1
_cell_length_a                   22.9056(6)
_cell_length_b                   24.2276(5)
_cell_length_c                   24.8145(6)
_cell_measurement_reflns_used    12864
_cell_measurement_temperature    123.6(5)
_cell_measurement_theta_max      29.1009
_cell_measurement_theta_min      2.8383
_cell_volume                     10867.6(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.6(5)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -3.00   87.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935   57.0000    0.0000 90

  2 omega  -51.00  -24.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935  -57.0000 -150.0000 27

  3 omega  -10.00   71.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935   77.0000   90.0000 81

  4 omega   34.00   95.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935 -178.0000 -120.0000 61

  5 omega  -12.00   35.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935   77.0000 -120.0000 47

  6 omega  -40.00   34.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935  -37.0000 -150.0000 74

  7 omega  -88.00  -47.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6622  -77.0000  120.0000 41
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0153774000
_diffrn_orient_matrix_UB_12      0.0122474000
_diffrn_orient_matrix_UB_13      0.0113093000
_diffrn_orient_matrix_UB_21      0.0272359000
_diffrn_orient_matrix_UB_22      0.0087038000
_diffrn_orient_matrix_UB_23      -0.0310278000
_diffrn_orient_matrix_UB_31      -0.0147335000
_diffrn_orient_matrix_UB_32      0.0296373000
_diffrn_orient_matrix_UB_33      -0.0126065000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.1474
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            80589
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.927
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             3190
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
The remaining solvent molecules were disordered and assigned as 7 DMSO and 67 MeOH molecules per unit cell, which were determined by SQUEEZE, TGA, and EA results. The contributions of these disordered solvent to the scattering values have been removed by using the PLATON SQUEEZE program. We can see from the SQUEEZE that some 1514 electrons were removed from the unit cell. The total formula unit should include 7 DMSO and 67 MeOH molecules (7*44e+67*18=1514).
;
_refine_diff_density_max         2.556
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1677
_refine_ls_number_reflns         38193
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19860
_reflns_number_total             38193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10815_si_004.cif
_cod_data_source_block           3D-cage-polymer
_cod_database_code               4129840
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_submission_special_instructions 'No special instructions were received'