DOSY NMR, X-ray Structural and Ion-Mobility Mass Spectrometric Studies on Electron-Deficient and Electron-Rich M6L4 Coordination Cages.
Bonakdarzadeh, Pia; Topić, Filip; Kalenius, Elina; Bhowmik, Sandip; Sato, Sota; Groessl, Michael; Knochenmuss, Richard; Rissanen, Kari; Inorganic chemistry 54 (2015) 6055–6061; doi:10.1021/acs.inorgchem.5b01082

data_4343103
_publ_section_title
;
 DOSY NMR, X-ray Structural and Ion-Mobility Mass Spectrometric Studies on
 Electron-Deficient and Electron-Rich M6L4 Coordination Cages.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6055
_journal_page_last               6061
_journal_paper_doi               10.1021/acs.inorgchem.5b01082
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C282 H240 N12 O12 P12 Pt6, 4(C F3 O3 S)'
_chemical_formula_sum            'C286 H240 F12 N12 O24 P12 Pt6 S4'
_chemical_formula_weight         6127.31
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                91.33(3)
_cell_angle_beta                 106.35(3)
_cell_angle_gamma                118.99(3)
_cell_formula_units_Z            2
_cell_length_a                   27.009(5)
_cell_length_b                   27.449(6)
_cell_length_c                   44.478(9)
_cell_measurement_temperature    293(2)
_cell_volume                     27171(15)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor 1997)'
_computing_data_collection       'KEK ugui'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris PILATUS 2M-F'
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.904
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.96000
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_Laue_measured_fraction_full 0.904
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            103698
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        29.999
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         1.167
_diffrn_source                   synchrotron
_diffrn_source_type              'KEK Photon Factory beamline BL1A'
_exptl_absorpt_coefficient_mu    2.341
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6104
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2617
_refine_ls_number_reflns         58156
_refine_ls_number_restraints     8292
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0649
_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^)+(0.1286P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1960
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                36074
_reflns_number_total             58156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01082_si_003.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 4343103--4343105.cif.'
_cod_original_cell_volume        27171(12)
_cod_database_code               4343103
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.387
_shelx_estimated_absorpt_t_max   0.892
_shelx_res_checksum              20659
_shelx_hkl_checksum              43166
_shelx_fab_checksum              30867