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_4129839
_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         'C320 H582 Cu24 O231.5 S16.5'
_chemical_formula_sum            'C320 H582 Cu24 O231.5 S16.5'
_chemical_formula_weight         10188.08
_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                64.384(6)
_cell_angle_beta                 61.760(6)
_cell_angle_gamma                87.652(4)
_cell_formula_units_Z            1
_cell_length_a                   24.4095(11)
_cell_length_b                   24.6581(15)
_cell_length_c                   25.0195(15)
_cell_measurement_reflns_used    13984
_cell_measurement_temperature    127.9(6)
_cell_measurement_theta_max      27.0060
_cell_measurement_theta_min      3.2390
_cell_volume                     11706.2(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      127.9(6)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    0.00   87.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   57.0000 -150.0000 87

  2 omega   44.00   79.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372 -130.0000  -99.5286 35

  3 omega    4.00   81.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   57.0000  120.0000 77

  4 omega  -51.00   37.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -57.0000  120.0000 88

  5 omega  -41.00   39.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -57.0000  -60.0000 80

  6 omega  -12.00   86.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   77.0000    0.0000 98

  7 omega  -20.00   60.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -99.0000   60.0000 80

  8 omega   -4.00   77.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   37.0000  -60.0000 81

  9 omega  -37.00   48.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185   57.0000 -120.0000 85
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0227259000
_diffrn_orient_matrix_UB_12      -0.0277431000
_diffrn_orient_matrix_UB_13      0.0258738000
_diffrn_orient_matrix_UB_21      -0.0072613000
_diffrn_orient_matrix_UB_22      0.0099265000
_diffrn_orient_matrix_UB_23      0.0248958000
_diffrn_orient_matrix_UB_31      -0.0238111000
_diffrn_orient_matrix_UB_32      0.0139474000
_diffrn_orient_matrix_UB_33      -0.0062100000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_av_unetI/netI     0.1354
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            143108
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.875
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             3244
_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 12 DMSO and 95 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 2234 electrons were removed from the unit cell. The total formula unit should include 12 DMSO and 95 MeOH molecules.
;
_refine_diff_density_max         1.320
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1492
_refine_ls_number_reflns         41201
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.1426
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1265P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2298
_refine_ls_wR_factor_ref         0.2581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18226
_reflns_number_total             41201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10815_si_003.cif
_cod_data_source_block           2D-cage-polymer
_cod_original_cell_volume        11706.2(14)
_cod_database_code               4129839
_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'