A Self-assembled M2L2 Truncated Square and its Application as a Container for Fullerenes
Yuan, Jun; Lv, Wanqian; Li, Anquan; Zhu, Kelong; Chemical Communications  (2021) –; doi:10.1039/D1CC05581J

data_7129207
_publ_section_title
;
 A Self-assembled M2L2 Truncated Square and its Application as a Container
 for Fullerenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05581J
_journal_year                    2021
_chemical_formula_sum            'C150 H156 F12 N4 O24 P4 Pt2 S12'
_chemical_formula_weight         3525.56
_chemical_name_systematic        Pt2(dppp)2(1)2(OTf)4
_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             2020-05-11
_audit_creation_method
;
FinalCif V69 by Daniel Kratzert, Freiburg 2019,
https://github.com/dkratzert/FinalCif
;
_audit_update_record
;
2021-10-01 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                103.6680(10)
_cell_angle_beta                 98.4290(10)
_cell_angle_gamma                104.3500(10)
_cell_formula_units_Z            1
_cell_length_a                   11.9342(2)
_cell_length_b                   17.2712(2)
_cell_length_c                   25.9639(3)
_cell_measurement_reflns_used    29106
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.9260
_cell_measurement_theta_min      4.0500
_cell_volume                     4916.75(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;

List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -120.00   0.00   1.00    2.00    --  -40.77 -19.00 -90.00  120
  2  \w    -75.00  -6.00   1.00    2.00    --  -40.77 125.00   0.00   69
  3  \w   -113.00 -38.00   1.00    2.00    --  -40.77 -38.00-150.00   75
  4  \w      1.00  79.00   1.00    2.00    --   40.77 -99.00-180.00   78
  5  \w     39.00  85.00   1.00    2.00    --   40.77-125.00   0.00   46
  6  \w     23.00  53.00   1.00    2.00    --   40.77-125.00-180.00   30
  7  \w     65.00 100.00   1.00    8.00    --  112.00-111.00 120.00   35
  8  \w     38.00  76.00   1.00    8.00    --  112.00-111.00  30.00   38
  9  \w     85.00 123.00   1.00    8.00    --  112.00 -61.00 -60.00   38
 10  \w     75.00 110.00   1.00    8.00    --  112.00 -94.00-180.00   35
 11  \w     88.00 113.00   1.00    8.00    --  112.00-111.00  90.00   25
 12  \w     79.00 108.00   1.00    8.00    --  112.00-111.00  30.00   29
 13  \w     69.00 113.00   1.00    8.00    --  112.00-111.00 150.00   44
 14  \w     97.00 124.00   1.00    8.00    --  112.00 178.00  30.00   27
 15  \w     74.00 100.00   1.00    8.00    --  112.00-111.00   0.00   26
 16  \w    117.00 145.00   1.00    8.00    --  112.00 111.00  30.00   28
 17  \w     63.00 178.00   1.00    8.00    --  112.00  15.00 150.00  115
 18  \w     84.00 163.00   1.00    8.00    --  112.00  61.00-180.00   79
 19  \w    118.00 147.00   1.00    8.00    --  112.00  77.00-150.00   29
 20  \w    122.00 178.00   1.00    8.00    --  112.00  77.00 150.00   56
 21  \w     42.00  89.00   1.00    8.00    --  112.00 -45.00  60.00   47
 22  \w     36.00  75.00   1.00    8.00    --  112.00-111.00  90.00   39
 23  \w     37.00 113.00   1.00    8.00    --  112.00-111.00-180.00   76
 24  \w     60.00 159.00   1.00    8.00    --  112.00  15.00 -60.00   99
 25  \w     53.00 141.00   1.00    8.00    --  112.00 -61.00  90.00   88
 26  \w     36.00  79.00   1.00    8.00    --  112.00 -30.00 -90.00   43
 27  \w    114.00 139.00   1.00    8.00    --  112.00 -30.00 -90.00   25
 28  \w     66.00 113.00   1.00    8.00    --  112.00-111.00 -60.00   47
 29  \w     47.00 136.00   1.00    8.00    --  112.00 -45.00-180.00   89
 30  \w     95.00 144.00   1.00    8.00    --  112.00 -77.00 -30.00   49
 31  \w     70.00 108.00   1.00    8.00    --  112.00-111.00 -90.00   38
 32  \w    109.00 134.00   1.00    8.00    --  112.00  61.00 -90.00   25
 33  \w     37.00  92.00   1.00    8.00    --  112.00-111.00-120.00   55
 34  \w     67.00 113.00   1.00    8.00    --  112.00-111.00 -30.00   46
 35  \w     45.00  76.00   1.00    8.00    --  112.00 -61.00 -60.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1298750000
_diffrn_orient_matrix_UB_12      0.0440032000
_diffrn_orient_matrix_UB_13      0.0011148000
_diffrn_orient_matrix_UB_21      -0.0409980000
_diffrn_orient_matrix_UB_22      0.0596414000
_diffrn_orient_matrix_UB_23      -0.0289494000
_diffrn_orient_matrix_UB_31      0.0095576000
_diffrn_orient_matrix_UB_32      0.0610751000
_diffrn_orient_matrix_UB_33      0.0554566000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            51826
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.248
_diffrn_reflns_theta_min         3.590
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.668
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent light colourless'
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.380
_refine_diff_density_max         3.279
_refine_diff_density_min         -3.048
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         20261
_refine_ls_number_restraints     1356
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0893P)^2^+17.0720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1898
_refine_ls_wR_factor_ref         0.1952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18612
_reflns_number_total             20261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05581j2.cif
_cod_data_source_block           a20051101a0089_a_sq
_cod_original_cell_volume        4916.74(12)
_cod_database_code               7129207
_shelx_shelxl_version_number     2018/3
_cell_oxdiff_length_a            11.9342(2)
_cell_oxdiff_length_b            17.2712(2)
_cell_oxdiff_length_c            25.9639(2)
_cell_oxdiff_angle_alpha         103.6682(9)
_cell_oxdiff_angle_beta          98.4295(12)
_cell_oxdiff_angle_gamma         104.3499(14)
_cell_oxdiff_volume              4916.73(13)
_cell_oxdiff_measurement_reflns_used 29106
_oxdiff_exptl_absorpt_empirical_full_min 0.325
_oxdiff_exptl_absorpt_empirical_full_max 1.711
_oxdiff_exptl_absorpt_empirical_details
;

Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_ac3_digest_frames
;
01627e2dba76b158fe7c5ef6949c24864c000337929
;
_diffrn_oxdiff_ac3_digest_hkl
;
019967044a43fd0fde0690a58ae611ef402823
;
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_theta     74.33
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         C34H28N3S4F6O6PtP2
_chemical_oxdiff_usercomment     S-DPPP-Pt
_shelx_res_checksum              18832
_shelx_fab_checksum              6942