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_7129206
_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            'C186 H108 F12 N4 O12 P4 Pt2 S12'
_chemical_formula_weight         3717.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-06-22
_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                90
_cell_angle_beta                 103.070(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.3955(6)
_cell_length_b                   17.1804(3)
_cell_length_c                   35.9313(7)
_cell_measurement_reflns_used    19562
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.5300
_cell_measurement_theta_min      4.3290
_cell_volume                     23088.1(7)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -85.00  37.00   1.00   20.00    --  -41.14   0.00 -60.00  122
  2  \w     27.00  85.00   1.00   20.00    --   41.14-125.00-120.00   58
  3  \w     34.00  78.00   1.00   20.00    --   41.14-125.00  90.00   44
  4  \w     37.00 109.00   1.00   80.00    --  112.00 -94.00  60.00   72
  5  \w     45.00  70.00   1.00   80.00    --  112.00-125.00-150.00   25
  6  \w     33.00 105.00   1.00   80.00    --  112.00 -94.00 -90.00   72
  7  \w     72.00 141.00   1.00   80.00    --  112.00 -61.00  30.00   69
  8  \w    125.00 174.00   1.00   80.00    --  112.00  93.00 140.00   49
  9  \w     81.00 175.00   1.00   80.00    --  112.00  15.00 150.00   94
 10  \w    107.00 174.00   1.00   80.00    --  112.00  45.00  30.00   67
 11  \w     32.00  64.00   1.00   40.00    --   41.14-125.00-180.00   32
 12  \w     44.00  70.00   1.00  160.00    --  112.00-125.00-150.00   26
 13  \w     45.00  71.00   1.00  160.00    --  112.00-125.00 -90.00   26
 14  \w   -115.00 -17.00   1.00   40.00    --  -41.14 -38.00-150.00   98
;
_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      0.0378830000
_diffrn_orient_matrix_UB_12      -0.0074488000
_diffrn_orient_matrix_UB_13      -0.0073354000
_diffrn_orient_matrix_UB_21      -0.0090069000
_diffrn_orient_matrix_UB_22      -0.0825814000
_diffrn_orient_matrix_UB_23      -0.0160313000
_diffrn_orient_matrix_UB_31      -0.0134880000
_diffrn_orient_matrix_UB_32      0.0340251000
_diffrn_orient_matrix_UB_33      -0.0403340000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1028
_diffrn_reflns_av_sigmaI/netI    0.1153
_diffrn_reflns_av_unetI/netI     0.1145
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            47273
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.589
_diffrn_reflns_theta_max         66.589
_diffrn_reflns_theta_min         3.612
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30776
_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_density_diffrn    1.069
_exptl_crystal_description       block
_exptl_crystal_F_000             7456
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.208
_refine_diff_density_min         -2.110
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1365
_refine_ls_number_reflns         20276
_refine_ls_number_restraints     14006
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.1627
_refine_ls_R_factor_gt           0.1267
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+820.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3068
_refine_ls_wR_factor_ref         0.3249
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13601
_reflns_number_total             20276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05581j2.cif
_cod_data_source_block           exp_786_a_sq
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7129206
_shelx_shelxl_version_number     2018/3
_cell_oxdiff_length_a            38.3791(8)
_cell_oxdiff_length_b            17.1882(4)
_cell_oxdiff_length_c            35.9322(8)
_cell_oxdiff_angle_alpha         90.0902(19)
_cell_oxdiff_angle_beta          103.0820(18)
_cell_oxdiff_angle_gamma         90.0287(18)
_cell_oxdiff_volume              23088.1(9)
_cell_oxdiff_measurement_reflns_used 19633
_oxdiff_exptl_absorpt_empirical_full_min 0.544
_oxdiff_exptl_absorpt_empirical_full_max 2.086
_oxdiff_exptl_absorpt_empirical_details
;

Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_ac3_digest_frames
;
01b4ba7d828ef547e35d50ad4bd6c9cbeb00702203e
;
_diffrn_oxdiff_ac3_digest_hkl
;
011be3531cd6f6a7e280b0d3cb659f9111e438
;
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_theta     68.13
_reflns_odcompleteness_iscentric 1
_shelx_res_checksum              50192
_shelx_fab_checksum              72047