Novel molybdenum(V) squarato complexes based on the dinuclear metal‒metal bonded unit: syntheses and structural characterization of dinuclear [Mo2O4(C4O4)(R-Py)4] and tetranuclear [Mo4O8(C4O4)4]4−
Barbara Modec; Jurij V. Brenčič; Eric M. Burkholder; Jon Zubieta; Dalton Trans.  (2003) 4618–4625; doi:10.1039/b311348e

data_7013662
_publ_section_title
;
 Novel molybdenum(V) squarato complexes based on the dinuclear
 metal--metal bonded unit: syntheses and structural characterization of
 dinuclear [Mo2O4(C4O4)(R-Py)4] and tetranuclear
 [Mo4O8(C4O4)4]4&#x2212;
;
_journal_issue                   24
_journal_name_full               'Dalton Trans.'
_journal_page_first              4618
_journal_page_last               4625
_journal_paper_doi               10.1039/b311348e
_journal_year                    2003
_chemical_formula_sum            'C46 H54 Mo2 N6 O8'
_chemical_formula_weight         1010.83
_chemical_name_common
;Tetra(3,5-lutidine)tetraoxosquaratodimolybdenum(V) (3,5-
lutidine) (1/2)
;
_chemical_name_systematic
;
Tetra(3,5-lutidine)tetraoxosquaratodimolybdenum(V)
(3,5-lutidine) (1/2)
;
_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                90.3260(10)
_cell_angle_beta                 92.4660(10)
_cell_angle_gamma                111.8640(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9594(5)
_cell_length_b                   11.8057(6)
_cell_length_c                   21.0573(11)
_cell_measurement_temperature    90(2)
_cell_volume                     2295.0(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Phi and omega scan'
_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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29617
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.343
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         14929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+1.4189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                13130
_reflns_number_total             14929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b311348e.txt
_cod_data_source_block           1c
_cod_database_code               7013662