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_4326897
_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            'C20 H70 Mo6 N20 O40 P4'
_chemical_formula_weight         1930.48
_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                81.723(2)
_cell_angle_beta                 79.307(2)
_cell_angle_gamma                78.468(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2994(4)
_cell_length_b                   12.5679(4)
_cell_length_c                   19.8205(6)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.58
_cell_volume                     2693.25(15)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            86914
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    1.604
_exptl_absorpt_correction_T_max  0.8259
_exptl_absorpt_correction_T_min  0.4067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_description       block
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.414
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.179
_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     371
_refine_ls_number_reflns         10831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0700P)^2^+26.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1579
_reflns_number_gt                8641
_reflns_number_total             10831
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201652h_si_005.cif
_cod_data_source_block           ab42
_cod_database_code               4326897