A hybrid bimetallic complex from regioselective <i>in situ</i> ligand oxidation: poly[(μ-β-octamolybdato-κ^2^<i>O</i>:<i>O</i>)bis[μ-4-(2-pyridyl)pyridinium-3-olato-κ^3^<i>N</i>,<i>O</i>:<i>O</i>]bis[4-(2-pyridyl)pyridinium-3-olato-κ^2^<i>N</i>,<i>O</i>]dicopper(II)]
Springsteen, Caleb H.; Rarig Jr, Randy S.; Zubieta, Jon; LaDuca, Robert L.; Acta Crystallographica Section E 63 (2007) m933–m935; doi:10.1107/S1600536807009282

data_2212877
_publ_section_title
;A hybrid bimetallic complex from regioselective <i>in situ</i> ligand
 oxidation:
 poly[(\m-\b-octamolybdato-\k^2^<i>O</i>:<i>O</i>)bis[\m-4-(2-pyridyl)pyridinium-3-olato-\k^3^<i>N</i>,<i>O</i>:<i>O</i>]bis[4-(2-pyridyl)pyridinium-3-olato-\k^2^<i>N</i>,<i>O</i>]dicopper(II)]
;
_journal_coeditor_code           GK2058
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m933
_journal_page_last               m935
_journal_paper_doi               10.1107/S1600536807009282
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cu2 Mo8 O26 (C10 H8 N2 O)4]'
_chemical_formula_moiety         'C40 H32 Cu2 Mo8 N8 O30'
_chemical_formula_sum            'C40 H32 Cu2 Mo8 N8 O30'
_chemical_formula_weight         1999.34
_chemical_name_systematic
;
poly[(\m-\b-octamolybdato-\k^2^O:O)bis[\m-4-(2-pyridyl)pyridinium-3-olato-
\k^3^N,O:O]bis[4-(2-pyridyl)pyridinium-3-olato-\k^2^N:O]dicopper(II)]
;
_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           SHELXL97
_cell_angle_alpha                100.607(2)
_cell_angle_beta                 107.197(2)
_cell_angle_gamma                102.838(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9620(13)
_cell_length_b                   10.1592(13)
_cell_length_c                   13.7049(17)
_cell_measurement_reflns_used    15331
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      1.61
_cell_volume                     1244.6(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2003)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2005)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker SMART 1K'
_diffrn_measurement_method       \w
_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  0.0815
_diffrn_reflns_av_sigmaI/netI    0.1291
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15331
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.890
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             962
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.236
_refine_diff_density_min         -1.148
_refine_ls_extinction_coef       0.0046(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5925
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1284
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0592P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                3211
_reflns_number_total             5925
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gk2058.cif
_cod_data_source_block           I
_cod_database_code               2212877
_cod_database_fobs_code          2212877