Aftermath of irradiation: the stacking faults in crystal of giant supramolecule unexpectedly mended before total decay
Peresypkina, Eugenia; Stöger, Berthold; Virovets, Alexander; CrystEngComm  (2022) –; doi:10.1039/D2CE00916A

data_7245603
_publ_section_title
;
 Aftermath of irradiation: the stacking faults in crystal of giant
 supramolecule unexpectedly mended before total decay
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00916A
_journal_year                    2022
_chemical_formula_moiety
'C150 H210 Cu14 I14 O20 P40 Ta10, (C2 H3 N)4.80'
_chemical_formula_structural
'[((C13 H21) Ta P4 (C O)2)10 (Cu I)14] * 4.8MeCN'
_chemical_formula_sum            'C159.6 H224.4 Cu14 I14 N4.8 O20 P40 Ta10'
_chemical_formula_weight         8244.69
_chemical_properties_physical
'Air-sensitive,Moisture-sensitive,Efflorescent,X-ray sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-03 deposited with the CCDC.	2022-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.718(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   32.9341(14)
_cell_length_b                   26.3182(14)
_cell_length_c                   20.9738(7)
_cell_measurement_reflns_used    9008
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      71.7960
_cell_measurement_theta_min      4.2010
_cell_volume                     14572.4(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1998)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25766
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         73.714
_diffrn_reflns_theta_min         4.221
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.795
_exptl_absorpt_correction_T_max  0.497
_exptl_absorpt_correction_T_min  0.327
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'orange to brown'
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_description       prism
_exptl_crystal_F_000             7707
_exptl_crystal_size_max          0.067
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.042
_refine_diff_density_max         4.579
_refine_diff_density_min         -2.575
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         14128
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1427P)^2^+117.0442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2283
_refine_ls_wR_factor_ref         0.2431
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9310
_reflns_number_total             14128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00916a2.cif
_cod_data_source_block           sm2ne
_cod_original_cell_volume        14572.3(12)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C159.60 H224.40 Cu14 I14 N4.80 O20 P40 Ta10'
_cod_database_code               7245603
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.653
_oxdiff_exptl_absorpt_empirical_full_max 1.541
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              30225