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_1551165
_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         'C198 H145 Cu24 O139 S'
_chemical_formula_sum            'C198 H145 Cu24 O139 S'
_chemical_formula_weight         6305.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                88.010(2)
_cell_angle_beta                 79.070(3)
_cell_angle_gamma                75.949(3)
_cell_formula_units_Z            2
_cell_length_a                   24.5209(10)
_cell_length_b                   25.3703(7)
_cell_length_c                   37.0128(12)
_cell_measurement_reflns_used    8055
_cell_measurement_temperature    128.40(14)
_cell_measurement_theta_max      20.2850
_cell_measurement_theta_min      3.1430
_cell_volume                     21930.1(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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      128.40(14)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.576
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -53.00   57.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8810  -19.0000    0.0000 110

  2 omega    0.00   60.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8810  -99.0000   60.0000 60

  3 omega   24.00   60.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8810  -99.0000  -60.0000 36

  4 omega   35.00   81.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8810 -178.0000 -180.0000 46

  5 omega   35.00   94.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8810 -178.0000   30.0000 59

  6 omega    1.00   29.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8810  -37.0000 -120.0000 28

  7 omega  -11.00   74.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8810   77.0000 -180.0000 85

  8 omega  -31.00   44.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8810  -19.0000  -90.0000 75

  9 omega  -35.00    7.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6622  -77.0000 -180.0000 42
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0177577000
_diffrn_orient_matrix_UB_12      -0.0199973000
_diffrn_orient_matrix_UB_13      0.0093060000
_diffrn_orient_matrix_UB_21      -0.0214405000
_diffrn_orient_matrix_UB_22      0.0046686000
_diffrn_orient_matrix_UB_23      0.0161461000
_diffrn_orient_matrix_UB_31      -0.0120950000
_diffrn_orient_matrix_UB_32      -0.0202246000
_diffrn_orient_matrix_UB_33      -0.0058048000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1366
_diffrn_reflns_av_unetI/netI     0.2385
_diffrn_reflns_Laue_measured_fraction_full 0.576
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            138592
_diffrn_reflns_point_group_measured_fraction_full 0.576
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.816
_diffrn_reflns_theta_min         2.775
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.201
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    0.955
_exptl_crystal_description       block
_exptl_crystal_F_000             6314
_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 18 DMSO and 66 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 3962 electrons were removed from the unit cell, that is, some 3962/2 = 1981 electrons per formula unit.  The total formula unit should include 18 DMSO and 66 MeOH molecules (18*44e+66*18=1980).
;
_refine_diff_density_max         1.356
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.841
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2634
_refine_ls_number_reflns         45715
_refine_ls_number_restraints     513
_refine_ls_restrained_S_all      0.845
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.0840
_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^)+(0.0809P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1970
_refine_ls_wR_factor_ref         0.2263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18111
_reflns_number_total             45715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01892a2.cif
_cod_data_source_block           2
_cod_database_code               1551165
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         C1Cu1
_reflns_odcompleteness_completeness 50.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_submission_special_instructions 'No special instructions were received'