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_4343104
_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         'C270 H204 F12 N12 P12 Pt6'
_chemical_formula_sum            'C270 H204 F12 N12 P12 Pt6'
_chemical_formula_weight         5386.62
_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                82.93(3)
_cell_angle_beta                 74.48(3)
_cell_angle_gamma                75.43(3)
_cell_formula_units_Z            2
_cell_length_a                   27.774(6)
_cell_length_b                   30.851(6)
_cell_length_c                   33.238(7)
_cell_measurement_temperature    293(2)
_cell_volume                     26512(11)
_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 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.96000
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            69517
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.850
_diffrn_reflns_theta_max         25.850
_diffrn_reflns_theta_min         1.223
_diffrn_source                   synchrotron
_diffrn_source_type              'KEK Photon Factory beamline BL1A'
_exptl_absorpt_coefficient_mu    2.342
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5328
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2209
_refine_ls_number_reflns         38674
_refine_ls_number_restraints     7788
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0686
_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^)+(0.1660P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2368
_refine_ls_wR_factor_ref         0.2503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27687
_reflns_number_total             38674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01082_si_004.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 4343103--4343105.cif.'
_cod_database_code               4343104
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.540
_shelx_estimated_absorpt_t_max   0.652
_shelx_res_checksum              36875
_shelx_hkl_checksum              82957
_shelx_fab_checksum              52362