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_4325685
_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 N8 O21 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C72 H106 N10 O21 V6'
_chemical_formula_weight         1753.31
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 110.398(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   43.2834(12)
_cell_length_b                   16.4677(5)
_cell_length_c                   16.4447(5)
_cell_measurement_reflns_used    22742
_cell_measurement_temperature    200
_cell_measurement_theta_max      71.91
_cell_measurement_theta_min      2.18
_cell_volume                     10986.4(6)
_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 5.5
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Smart 6000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Montel 200 optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            72898
_diffrn_reflns_theta_full        72.75
_diffrn_reflns_theta_max         72.75
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    4.575
_exptl_absorpt_correction_T_max  0.4809
_exptl_absorpt_correction_T_min  0.2996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_description       block
_exptl_crystal_F_000             3656
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
Attempts to  model disordered solvent molecules
were unsuccessful. PLATON/SQUEEZE  was used to correct
the data for the presence of the disordered solvent.
A potential solvent volume of 3584.3 \%A^3^, 
32.6 % of the total unit-cell volume, was found.
878 electrons per unit cell worth of scattering were located
in the void. The reported structure is based on the 
PLATON/SQUEEZE corrected data. The actual solvent content is
unknown, so several quantities calculated like empirical formula, density, 
absorption coefficient, F(000) etc. may be incorrect.

Ref:  Sluis, P. van der & Spek, A.L. (1990). Acta Cryst. A46, 194-201.
;
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         10854
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.161
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1122P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1580
_reflns_number_gt                8548
_reflns_number_total             10854
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic200752v_si_003.cif
_cod_data_source_block           mper16
_cod_database_code               4325685