From 0D dimer to 2D Network-Supramolecular Assembly of Organic Derivatized Polyoxometalates with Remote Hydroxyl via Hydrogen Bonding
Longsheng Wang; Li Zhu; Panchao Yin; Weiwei Fu; Jiake Chen; Jian Hao; Fengping Xiao; Chunlin Lv; Jin Zhang; Lu Shi; Qiang Li; Yongge Wei; Inorganic Chemistry 48 (2009) 9222–9235; doi:10.1021/ic900985w

data_4303237
_publ_contact_author_address
;
Department of Chemistry
Tsinghua University
Beijing 100084
P. R. China
;
_publ_contact_author_email       yonggewei@mail.tsinghua.edu.cn
_publ_contact_author_name        'Dr Yongge Wei'
_publ_section_title
;
From 0D dimer to 2D Network-Supramolecular Assembly of Organic
Derivatized Polyoxometalates with Remote Hydroxyl via Hydrogen Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9222
_journal_page_last               9235
_journal_paper_doi               10.1021/ic900985w
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C40 H83 Mo6 N3 O20'
_chemical_formula_weight         1501.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.63(3)
_cell_angle_beta                 72.36(3)
_cell_angle_gamma                79.75(3)
_cell_formula_units_Z            2
_cell_length_a                   12.604(3)
_cell_length_b                   13.104(3)
_cell_length_c                   19.371(4)
_cell_measurement_reflns_used    15565
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.94
_cell_measurement_theta_min      6.21
_cell_volume                     2910.3(13)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '100x100 micron'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       Oscillation
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25111
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.321
_exptl_absorpt_correction_T_max  0.6201
_exptl_absorpt_correction_T_min  0.4180
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.086
_refine_diff_density_min         -1.481
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         11380
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0620P)^2^+1.6474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                9352
_reflns_number_total             11380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900985w_si_001_5.cif
_cod_data_source_block           Phen-EtOH
_cod_original_cell_volume        2910.3(10)
_cod_database_code               4303237