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_7054983
_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
' (O2 N O C3 H6 N Mo6 O18), (C3 H6 N Mo6 O18), 4(C16 H36 N)'
_chemical_formula_sum            'C35 H78 Cl0.5 Mo6 N3.5 O19.5'
_chemical_formula_weight         1453.37
_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                   16.779(3)
_cell_length_b                   20.069(4)
_cell_length_c                   31.884(6)
_cell_measurement_reflns_used    74311
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      3.00
_cell_volume                     10737(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 0.997
_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  0.0542
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            81646
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.006
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.452
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS, Sheldrick 1996)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5832
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.391
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         10533
_refine_ls_number_restraints     361
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0481P)^2^+36.4390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1343
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8540
_reflns_number_total             10533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj01090j2.cif
_cod_data_source_block           Compound-3
_cod_depositor_comments
'Adding full bibliography for 7054981--7054983.cif.'
_cod_original_formula_sum        'C35 H78 Cl0.50 Mo6 N3.50 O19.50'
_cod_database_code               7054983
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.530
_shelx_estimated_absorpt_t_max   0.670
_shelx_res_checksum              19956