An Inclusion Complex of Hexamolybdate inside a Supramolecular Cage and Its Structural Conversion
Muxin Han; Jakob Hey; Wataru Kawamura; Dietmar Stalke; Mitsuhiko Shionoya; Guido H. Clever; Inorganic Chemistry 51 (2012) 9574–9576; doi:10.1021/ic301359n

data_4330377
_publ_section_title
;
 An Inclusion Complex of Hexamolybdate inside a Supramolecular Cage and
 Its Structural Conversion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9574
_journal_page_last               9576
_journal_paper_doi               10.1021/ic301359n
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C138.7 H102.05 F18 Mo6 N21.35 O34'
_chemical_formula_weight         3529.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                62.61(2)
_cell_angle_beta                 82.90(2)
_cell_angle_gamma                73.80(2)
_cell_formula_units_Z            2
_cell_length_a                   14.986(4)
_cell_length_b                   23.994(8)
_cell_length_c                   24.610(9)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      21.726
_cell_measurement_theta_min      2.322
_cell_volume                     7545(5)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.4-1'
_computing_data_reduction        'SAINT V7.46A'
_computing_molecular_graphics    'ShelXle rev.489'
_computing_publication_material  'ShelXle rev.489'
_computing_structure_refinement  'SHELXL in SHELXTL Version 2008/3'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/3'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 SMART Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            119820
_diffrn_reflns_theta_full        23.14
_diffrn_reflns_theta_max         23.14
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'TWINABS 2008/4'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       block
_exptl_crystal_F_000             3546
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2144
_refine_ls_number_reflns         21239
_refine_ls_number_restraints     666
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+23.7442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                14577
_reflns_number_total             21239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301359n_si_002.cif
_cod_data_source_block           twin5
_cod_original_cell_volume        7545(4)
_cod_original_formula_sum        'C138.70 H102.05 F18 Mo6 N21.35 O34'
_cod_database_code               4330377