Bis[(1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')bis(triphenylphosphane-κ<i>P</i>)copper(I)] nonadecaoxidohexamolybdate(VI)
Gschwind, Fabienne; Jansen, Martin; Acta Crystallographica Section E 68 (2012) m1206–m1207; doi:10.1107/S1600536812036367

data_2236305
_publ_section_title
;
 Bis[(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')bis(triphenylphosphane-\k<i>P</i>)copper(I)]
 nonadecaoxidohexamolybdate(VI)
;
_journal_coeditor_code           HG5234
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1206
_journal_page_last               m1207
_journal_paper_doi               10.1107/S1600536812036367
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu (C12 H8 N2) (C18 H15 P)2]2 [Mo6 O19]'
_chemical_formula_moiety         '2(C48 H38 Cu N2 P2 +), Mo6 O19 2-'
_chemical_formula_sum            'C96 H76 Cu2 Mo6 N4 O19 P4'
_chemical_formula_weight         2416.23
_chemical_name_systematic
;
Bis[(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')bis(triphenylphosphane-
\k<i>P</i>)copper(I)] nonadecaoxidohexamolybdate(VI)
;
_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                109.03(3)
_cell_angle_beta                 102.98(3)
_cell_angle_gamma                93.93(3)
_cell_formula_units_Z            1
_cell_length_a                   11.287(2)
_cell_length_b                   13.572(3)
_cell_length_c                   16.307(3)
_cell_measurement_reflns_used    22955
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.7
_cell_measurement_theta_min      1.3
_cell_volume                     2273.7(10)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2009)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2009)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0307
_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       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22882
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    1.401
_exptl_absorpt_correction_T_max  0.9084
_exptl_absorpt_correction_T_min  0.8176
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 2009)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1202
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.565
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         9593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0449P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0630
_reflns_number_gt                7714
_reflns_number_total             9593
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hg5234.cif
_cod_data_source_block           I
_cod_original_cell_volume        2273.7(8)
_cod_database_code               2236305
_cod_database_fobs_code          2236305