Synthesis and characterisation of a lanthanide-capped dodecavanadate cage
Jamie M. Cameron; Graham N. Newton; Christoph Busche; De-Liang Long; Hiroki Oshio; Leroy Cronin; Chem.Commun. 49 (2013) 3395–; doi:10.1039/c3cc40912k

data_7109105
_publ_section_title
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 Synthesis and characterisation of a lanthanide-capped dodecavanadate cage
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_journal_name_full               Chem.Commun.
_journal_page_first              3395
_journal_paper_doi               10.1039/c3cc40912k
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C44 H94 Cl Gd N8 O34 V12'
_chemical_formula_weight         2083.26
_chemical_name_systematic
;
?
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.6592(14)
_cell_length_b                   25.175(2)
_cell_length_c                   10.2383(9)
_cell_measurement_reflns_used    6828
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      2.40
_cell_volume                     4036.1(6)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker Apex II Quasar CCD'
_diffrn_measurement_method       '\w & \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17042
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    2.240
_exptl_absorpt_correction_T_max  0.9157
_exptl_absorpt_correction_T_min  0.8070
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2086
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_platon_squeeze_details
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Summary and Remarks : N = NOTE, W = WARNING, E = ERROR
N: No S.U.'s (esd) on observed/calculated parameters.
N: DISORDERED structure - ATOMS with Pop. .LT. 1.0 are not moved or as a group.
W: Unit cell contains non-integral number of atoms (please check).
N: Number of Isotropic Non-H Atoms ....................................... 6
N: Number of moved primary input atoms: .................................. 9
N: Total Potential Solvent Accessible Void Vol .................. 262.7 Ang^3
N: Electron Count / Cell = 24 - To be included in D(calc), F000 & Mol.Wght.
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_refine_diff_density_max         0.91
_refine_diff_density_min         -0.49
_refine_diff_density_rms         0.10
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(11)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7447
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1011
_reflns_number_gt                6573
_reflns_number_total             7447
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3cc40912k.txt
_cod_data_source_block           jc149b
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_original_sg_symbol_H-M      P21212
_cod_original_formula_sum        'C44 H94 Cl1 Gd1 N8 O34 V12'
_cod_database_code               7109105