Propane-1,3-diylbis(triphenylphosphonium) (oxalato)oxodiperoxomolybdate(VI) monohydrate
Xian-Ying Shi; Jun-Fa Wei; Xi-Ru Zhang; Jing Cao; Acta Crystallographica Section E 63 (2007) m227–m229; doi:10.1107/S160053680605272X

data_2211861
_publ_section_title
;
 Propane-1,3-diylbis(triphenylphosphonium)
 (oxalato)oxodiperoxomolybdate(VI) monohydrate
;
_journal_coeditor_code           HY2033
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m227
_journal_page_last               m229
_journal_paper_doi               10.1107/S160053680605272X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C39 H36 P2) [Mo (C2 O4) O (O2)2], H2 O'
_chemical_formula_moiety         'C39 H36 P2, C2 Mo O9, H2 O'
_chemical_formula_sum            'C41 H38 Mo O10 P2'
_chemical_formula_weight         848.59
_chemical_name_systematic
;
Propane-1,3-diylbis(triphenylphosphonium) (oxalato)oxodiperoxomolybdate(VI)
monohydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.0400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9385(8)
_cell_length_b                   15.6425(12)
_cell_length_c                   11.8100(9)
_cell_measurement_reflns_used    6593
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      1.82
_cell_volume                     1910.2(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f and \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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9549
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  0.9304
_exptl_absorpt_correction_T_min  0.8517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             872.0
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.756
_refine_ls_abs_structure_details 'Flack (1983), 1458 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_coef       0.0132(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         6593
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0606P)^2^+3.2002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1509
_reflns_number_gt                5391
_reflns_number_total             6593
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2033.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2211861
_cod_database_fobs_code          2211861