Polyoxomolybdodiphosphonates: Examples Incorporating Ethylidenepyridines
Abhishek Banerjee; Farah S. Raad; Nina Vankova; Bassem S. Bassil; Thomas Heine; Ulrich Kortz; Inorganic Chemistry 50 (2011) 11667–11675; doi:10.1021/ic201652h

data_4326898
_publ_contact_author_address
;
School of Engineering and Science, Jacobs University, P.O. Box 750 561, 
28725 Bremen, Germany
;
_publ_contact_author_email       u.kortz@jacobs-university.de
_publ_contact_author_name        'Ulrich Kortz'
_publ_section_title
;
 Polyoxomolybdodiphosphonates: Examples Incorporating Ethylidenepyridines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11667
_journal_page_last               11675
_journal_paper_doi               10.1021/ic201652h
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C32 H72 Mo8 N16 Na8 O56 P8'
_chemical_formula_weight         2776.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   25.3368(11)
_cell_length_b                   25.3368(11)
_cell_length_c                   8.0896(4)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.09
_cell_measurement_theta_min      2.54
_cell_volume                     5193.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1020
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            119502
_diffrn_reflns_theta_full        24.75
_diffrn_reflns_theta_max         24.75
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_T_max  0.9542
_exptl_absorpt_correction_T_min  0.5868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       thread
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.366
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+30.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1771
_reflns_number_gt                3446
_reflns_number_total             4462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201652h_si_006.cif
_cod_data_source_block           ab43
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4326898