Discrete Covalent Organic-Inorganic Hybrids: Terpyridine Functionalized Polyoxometalates Obtained by a Modular Strategy and Their Metal Complexation
Marie-Pierre Santoni; Amlan K. Pal; Garry S. Hanan; Anna Proust; Bernold Hasenknopf; Inorganic Chemistry 50 (2011) 6737–6745; doi:10.1021/ic200752v

data_4325684
_publ_contact_author_address
;
      Universit\'e de Montr\'eal
      D\'epartement de Chimie
      C.P. 6128, Succ. Centre-ville
      Montr\'eal, Qu\'ebec
      Canada, H3C 3J7
;
_publ_contact_author_email       garry.hanan@umontreal.ca
_publ_contact_author_fax         '+1 514 343 7586'
_publ_contact_author_name        'Dr Garry S. Hanan'
_publ_contact_author_phone       '+1 514 343 7056'
_publ_section_title
;
 Discrete Covalent Organic-Inorganic Hybrids: Terpyridine Functionalized
 Polyoxometalates Obtained by a Modular Strategy and Their Metal
 Complexation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6737
_journal_page_last               6745
_journal_paper_doi               10.1021/ic200752v
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety
'C40 H34 Mn Mo6 N8 O26, 3(C16 H36 N), C4 H9 N O, C3 H7 N O'
_chemical_formula_sum            'C95 H158 Mn Mo6 N13 O28'
_chemical_formula_weight         2560.92
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 106.268(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4447(18)
_cell_length_b                   23.121(2)
_cell_length_c                   28.984(3)
_cell_measurement_reflns_used    60107
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.29
_cell_volume                     11222.3(19)
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection       'APEX2  (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'UdMX (Maris, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Graphite
_diffrn_radiation_source         'X-ray sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.110
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            283678
_diffrn_reflns_theta_full        26.26
_diffrn_reflns_theta_max         26.26
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.9512
_exptl_absorpt_correction_T_min  0.7927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       plate
_exptl_crystal_F_000             5280
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.781
_refine_diff_density_min         -1.337
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1263
_refine_ls_number_reflns         22654
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          4.999
_refine_ls_shift/su_mean         0.052
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1288P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1926
_refine_ls_wR_factor_ref         0.2134
_reflns_number_gt                13788
_reflns_number_total             22654
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic200752v_si_002.cif
_cod_data_source_block           mpier5
_cod_original_cell_volume        11222(2)
_cod_database_code               4325684