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_4326896
_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            'C19 H71 Mo4 N17 O37 P4'
_chemical_formula_weight         1637.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
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_symmetry_space_group_name_Hall  '-C 2yc'
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_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                 90.605(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.216(3)
_cell_length_b                   10.638(3)
_cell_length_c                   28.070(6)
_cell_measurement_reflns_used    9763
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.66
_cell_volume                     5439(2)
_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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            95272
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  0.8481
_exptl_absorpt_correction_T_min  0.2740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_description       block
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0350P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                5013
_reflns_number_total             5546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201652h_si_004.cif
_cod_data_source_block           c2c
_cod_database_code               4326896