N-alkylation of organo-imido substituted polyoxometalates: an efficient and stoichiometric approach for the easy post-modification of polyoxometalates.
Khan, Rao Naumaan Nasim; Lv, Chunlin; Zhang, Jin; Hao, Jian; Wei, Yongge; Dalton transactions (Cambridge, England : 2003) 44 (2015) 4568–4575; doi:10.1039/c4dt03637a

data_7033784
_publ_section_title
;
 N-alkylation of organo-imido substituted polyoxometalates: an efficient
 and stoichiometric approach for the easy post-modification of
 polyoxometalates.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4568
_journal_page_last               4575
_journal_paper_doi               10.1039/c4dt03637a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C45 H90 Mo6 N4 O19'
_chemical_formula_weight         1566.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-01-05 deposited with the CCDC.
2015-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.517(4)
_cell_length_b                   16.564(3)
_cell_length_c                   21.725(4)
_cell_measurement_reflns_used    10044
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.1297
_cell_measurement_theta_min      2.3305
_cell_volume                     6020(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device       'Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25663
_diffrn_reflns_theta_full        29.17
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_T_max  0.6961
_exptl_absorpt_correction_T_min  0.5321
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         12874
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                11376
_reflns_number_total             12874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03637a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7033784--7033786.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7033784