Use of a cyclo-P4 building block ‒ A Way to Networks of Host-Guest Assemblies
Scheer, Manfred; Presypkina, Eugenia V.; Virovets, Alexander Viktorovich; Bielmeier, Martin; Chemical Science  (2020) –; doi:10.1039/D0SC03437A

data_1558834
_publ_section_title
;
 Use of a cyclo-P4 building block -- A Way to Networks of Host-Guest
 Assemblies
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03437A
_journal_year                    2020
_chemical_formula_moiety
'P4 Se3, C160.5 H231 Ag8 N9 O16 P32 Ta8, 8(Sb F6), 3.75(C H 2 Cl2)'
_chemical_formula_structural
'(P4 Se3)@[{(C13 H21) Ta P4 (C O)2}8 Ag8 (N C(C H2)7 C N)4.5] * 3.75(C H2 Cl2)'
_chemical_formula_sum
'C164.25 H238.5 Ag8 Cl7.5 F48 N9 O16 P36 Sb8 Se3 Ta8'
_chemical_formula_weight         8409.36
_chemical_properties_physical
'Air-sensitive,Moisture-sensitive,Light-sensitive,X-ray sensitive'
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-06-15 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                81.1581(7)
_cell_angle_beta                 78.4160(7)
_cell_angle_gamma                73.7720(7)
_cell_formula_units_Z            2
_cell_length_a                   17.95491(12)
_cell_length_b                   22.56350(18)
_cell_length_c                   38.3495(4)
_cell_measurement_reflns_used    60540
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      31.3510
_cell_measurement_theta_min      1.7900
_cell_volume                     14534.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/5 (Sheldrick, 2018)'
_diffrn_ambient_temperature      80(2)
_diffrn_detector                 'pixel array detector'
_diffrn_detector_area_resol_mean 5.814
_diffrn_detector_type            'Dectris PILATUS 6M'
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device       'one-circle goniostat'
_diffrn_measurement_device_type
'P11 beamline, PETRA III, DESY, Dectris PILATUS 6M'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6888
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            144092
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        24.500
_diffrn_reflns_theta_max         24.835
_diffrn_reflns_theta_min         1.491
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    4.542
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.21a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_description       prism
_exptl_crystal_F_000             7969
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.680
_refine_diff_density_min         -4.676
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2830
_refine_ls_number_reflns         51920
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0895
_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^)+(0.1970P)^2^+22.2318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2777
_refine_ls_wR_factor_ref         0.2874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                43562
_reflns_number_total             51920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03437a2.cif
_cod_data_source_block           082
_cod_original_formula_sum
'C164.25 H238.50 Ag8 Cl7.50 F48 N9 O16 P36 Sb8 Se3 Ta8'
_cod_database_code               1558834
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.464
_shelx_estimated_absorpt_t_max   0.549
_oxdiff_exptl_absorpt_empirical_full_min 0.062
_oxdiff_exptl_absorpt_empirical_full_max 15.463
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_shelx_res_checksum              83849