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_1514522
_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 H155 Mn Mo6 N8 O29'
_chemical_formula_weight         2323.70
_chemical_name_systematic
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 ?
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_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   28.257(2)
_cell_length_b                   21.8128(16)
_cell_length_c                   16.5796(14)
_cell_measurement_reflns_used    8869
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2.36
_cell_volume                     10219.1(14)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker 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  0.0862
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            77882
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  0.9733
_exptl_absorpt_correction_T_min  0.8991
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
Summary and Remarks : N = NOTE, W = WARNING, E = ERROR
 
N: No S.U.'s (esd) on observed/calculated parameters.
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: Number of Isotropic Non-H Atoms .......................................   14
N: Number of moved primary input atoms: ..................................  132
N: Total Potential Solvent Accessible Void Vol ..................   683.0 Ang^3
N: Electron Count / Cell =    190 - To be included in D(calc), F000 & Mol.Wght.
 
;
_refine_diff_density_max         1.18
_refine_diff_density_min         -0.97
_refine_diff_density_rms         0.16
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         10308
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0823
_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^)+(0.1599P)^2^+12.9407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2554
_refine_ls_wR_factor_ref         0.2777
_reflns_number_gt                6182
_reflns_number_total             10308
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3sc51618k.txt
_cod_data_source_block           cy651b
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
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_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               1514522