A collection of robust methodologies for the preparation of asymmetric hybrid Mn‒Anderson polyoxometalates for multifunctional materials
Yvon, Carine; Macdonell, Andrew; Buchwald, Saskia; Surman, Andrew J.; Follet, Noémie; Alex, Jennifer; Long, De-Liang; Cronin, Leroy; Chemical Science 4 (2013) 3810–; doi:10.1039/c3sc51618k

data_1514521
_publ_section_title
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 A collection of robust methodologies for the preparation of asymmetric
 hybrid Mn--Anderson polyoxometalates for multifunctional materials
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_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3810
_journal_paper_doi               10.1039/c3sc51618k
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C80 H153 Mn Mo6 N8 O28'
_chemical_formula_weight         2305.68
_chemical_name_systematic
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 ? 
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 94.450(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.455(3)
_cell_length_b                   29.007(3)
_cell_length_c                   24.974(2)
_cell_measurement_reflns_used    9539
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.16
_cell_volume                     19829(3)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'ApexII 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  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            287148
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.02
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.9726
_exptl_absorpt_correction_T_min  0.8884
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9520
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
Summary and Remarks : N = NOTE, W = WARNING, E = ERROR
 
W: Coordinates do not form a Connected Set
N: DISORDERED structure - ATOMS with Pop. .LT. 1.0 are not moved or as a group.
N: No-Hydrogen atoms in this structure
N: Number of Isotropic Non-H Atoms .......................................   40
N: Number of moved primary input atoms: ..................................  288
W: Number of unusual anisotropic displacement parameters .................    4
N: Total Potential Solvent Accessible Void Vol ..................   999.3 Ang^3
N: Electron Count / Cell =    376 - To be included in D(calc), F000 & Mol.Wght.
 
;
_refine_diff_density_max         1.72
_refine_diff_density_min         -1.08
_refine_diff_density_rms         0.16
_refine_ls_extinction_coef       0.000036(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1854
_refine_ls_number_reflns         38952
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+309.6055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.1843
_reflns_number_gt                31801
_reflns_number_total             38952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc51618k.txt
_cod_data_source_block           nft141
_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      P2(1)/c
_cod_database_code               1514521