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_4129838
_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         'C407 H569 Cu24 N50 O201'
_chemical_formula_sum            'C407 H569 Cu24 N50 O201'
_chemical_formula_weight         10903.19
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.5211(7)
_cell_length_b                   26.5211(7)
_cell_length_c                   39.0679(16)
_cell_measurement_reflns_used    5719
_cell_measurement_temperature    128.9(3)
_cell_measurement_theta_max      25.7480
_cell_measurement_theta_min      3.3000
_cell_volume                     27479.1(15)
_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)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      128.9(3)
_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  -19.00   57.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -99.0000   30.0000 76

  2 omega    2.00   47.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -77.0000  -90.0000 45
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0038552000
_diffrn_orient_matrix_UB_12      0.0254764000
_diffrn_orient_matrix_UB_13      -0.0048438000
_diffrn_orient_matrix_UB_21      0.0159991000
_diffrn_orient_matrix_UB_22      -0.0035523000
_diffrn_orient_matrix_UB_23      -0.0143515000
_diffrn_orient_matrix_UB_31      -0.0210606000
_diffrn_orient_matrix_UB_32      -0.0073826000
_diffrn_orient_matrix_UB_33      -0.0100106000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.1010
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            28988
_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         25.009
_diffrn_reflns_theta_min         3.012
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88977
_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    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             6896
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_platon_squeeze_details
;
The remaining solvent molecules were disordered and assigned as 42 DMA and 15 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 4572 electrons were removed from the unit cell, that is, some 4572/2 = 2286 electrons per formula unit.  The total formula unit should include 42 DMA and 15 MeOH  molecules (42*48e+15*18=2286).
;
_refine_diff_density_max         2.315
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         12288
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1099P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.1991
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7210
_reflns_number_total             12288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10815_si_002.cif
_cod_data_source_block           0D-DMAcage
_cod_original_cell_volume        27479.1(18)
_cod_database_code               4129838
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_submission_special_instructions 'No special instructions were received'