Solvent-assisted coordination driven assembly of a supramolecular architecture featuring two types of connectivity from discrete nanocages
Niu, Zheng; Wang, Lei; Fang, Sheng; Lan, Pui Ching; Aguila, Briana; Perman, Jason A.; Ma, Jian-Gong; Cheng, Peng; Li, Xiaopeng; Ma, Shengqian; Chemical Science  (2019) –; doi:10.1039/C9SC01892A

data_1551164
_publ_section_title
;
 Solvent-assisted coordination driven assembly of a supramolecular
 architecture featuring two types of connectivity from discrete nanocages
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01892A
_journal_year                    2019
_chemical_formula_moiety         'C228 H204 Cu24 N12 O144'
_chemical_formula_sum            'C228 H204 Cu24 N12 O144'
_chemical_formula_weight         6940.98
_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'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-05-22 deposited with the CCDC.    2019-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.6201(10)
_cell_length_b                   28.6201(10)
_cell_length_c                   39.803(2)
_cell_measurement_reflns_used    4864
_cell_measurement_temperature    129.00(10)
_cell_measurement_theta_max      20.5200
_cell_measurement_theta_min      3.2230
_cell_volume                     32603(2)
_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, 2015)'
_diffrn_ambient_temperature      129.00(10)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega   29.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -99.0000  -30.0000 28

  2 omega  -26.00   33.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -37.0000 -150.0000 59

  3 omega   44.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  178.0000   30.0000 27

  4 omega  -41.00   42.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185   37.0000 -150.0000 83
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0170761000
_diffrn_orient_matrix_UB_12      -0.0179359000
_diffrn_orient_matrix_UB_13      -0.0004017000
_diffrn_orient_matrix_UB_21      -0.0109523500
_diffrn_orient_matrix_UB_22      0.0098061500
_diffrn_orient_matrix_UB_23      0.0143574500
_diffrn_orient_matrix_UB_31      -0.0142321500
_diffrn_orient_matrix_UB_32      0.0140097500
_diffrn_orient_matrix_UB_33      -0.0105590500
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1067
_diffrn_reflns_av_unetI/netI     0.1880
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            54494
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.871
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75395
_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    0.707
_exptl_crystal_description       block
_exptl_crystal_F_000             7008
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
The remaining solvent molecules were disordered and assigned as 59 DMF and 36 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 6033 electrons were removed from the unit cell, that is, some 6033/2 = 3016 electrons per formula unit. The total formula unit should include 59 DMF and 36 MeOH  molecules (59*40e+36*18=3008).
;
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         14507
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.1727
_refine_ls_R_factor_gt           0.0795
_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^)+(0.0940P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1971
_refine_ls_wR_factor_ref         0.2265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5010
_reflns_number_total             14507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01892a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        32603(3)
_cod_database_code               1551164
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         C1CU1
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_submission_special_instructions 'No special instructions were received'