Tris[bis(μ-1,10-phenanthrolin-2-olato)dicopper(I)] monosodium trihydrogen β-octamolybdate hemihydrate
Li, Ming-Xue; Ma, Peng-Tao; Wang, Jing-Ping; Acta Crystallographica Section E 62 (2006) m2661–m2663; doi:10.1107/S1600536806037433

data_2210506
_publ_section_title
;
 Tris[bis(\m-1,10-phenanthrolin-2-olato)dicopper(I)] monosodium
 trihydrogen \b-octamolybdate hemihydrate
;
_journal_coeditor_code           BI2061
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2661
_journal_page_last               m2663
_journal_paper_doi               10.1107/S1600536806037433
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'Na [H3 Mo8 O26] [Cu2 (C12 H7 N2 O)2]3, 0.5H2 O'
_chemical_formula_moiety
'3C24 H14 Cu2 N4 O2, H3 Mo8 O26 -, Na +, 0.5H2 O'
_chemical_formula_sum            'C72 H46 Cu6 Mo8 N12 Na O32.5'
_chemical_formula_weight         2770.98
_chemical_name_systematic
;
Tris[bis(\m-1,10-phenanthroline-2-olato)dicopper(I)]
monosodium trihydrogen \b-octamolybdate hemihydrate
;
_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                84.309(4)
_cell_angle_beta                 78.972(4)
_cell_angle_gamma                82.091(2)
_cell_formula_units_Z            1
_cell_length_a                   9.640(4)
_cell_length_b                   13.651(4)
_cell_length_c                   15.952(5)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     2035.1(12)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10029
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.818
_exptl_absorpt_correction_T_max  0.657
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.282
_refine_diff_density_min         -0.988
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         6828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0899P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.1586
_reflns_number_gt                4626
_reflns_number_total             6828
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi2061.cif
_cod_data_source_block           I
_cod_original_cell_volume        2035.1(11)
_cod_original_formula_sum        'C72 H46 Cu6 Mo8 N12 Na O32.50'
_cod_database_code               2210506
_cod_database_fobs_code          2210506