Nucleophilic substitution reaction for rational post-functionalization of polyoxometalates
Li, Qiang; Zhang, Jin; Wang, Longsheng; Hao, Jian; Yin, Panchao; Wei, Yongge; New J. Chem. 40 (2016) 906–; doi:10.1039/C5NJ01090J

data_7054981
_publ_section_title
;
 Nucleophilic substitution reaction for rational post-functionalization of
 polyoxometalates
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              906
_journal_paper_doi               10.1039/C5NJ01090J
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         '  (Cl C3 H6 N Mo6 O18), 2(C16 H36 N)'
_chemical_formula_sum            'C35 H78 Cl Mo6 N3 O18'
_chemical_formula_weight         1440.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-06-14 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.709(3)
_cell_length_b                   20.059(4)
_cell_length_c                   31.916(6)
_cell_measurement_reflns_used    67693
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     10697(4)
_computing_cell_refinement       'Rigaku RAPID AUTO Ver2.30'
_computing_data_collection       'Rigaku RAPID AUTO Ver2.30'
_computing_data_reduction        'Rigaku RAPID AUTO Ver2.30'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean '100x100 micron'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            80216
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.006
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.479
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS, Sheldrick 1996)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_description       block
_exptl_crystal_F_000             5776
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.404
_refine_diff_density_min         -1.504
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         10484
_refine_ls_number_restraints     350
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+44.2836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8423
_reflns_number_total             10484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj01090j2.cif
_cod_data_source_block           Compound-1
_cod_depositor_comments
'Adding full bibliography for 7054981--7054983.cif.'
_cod_database_code               7054981
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.665
_shelx_estimated_absorpt_t_max   0.756
_shelx_res_checksum              29591