Investigation of induction times, activity, selectivity, interface and mass transport in solvent-free epoxidation by H2O2 and TBHP: a study with organic salts of the [PMo12O40]3− anion
Guérin, Béatrice; Fernandes, Daniel Mesquita; Daran, Jean-Claude; Agustin, Dominique; Poli, Rinaldo; New Journal of Chemistry 37 (2013) 3466–; doi:10.1039/c3nj00523b

data_7053187
_publ_section_title
;
 Investigation of induction times, activity, selectivity, interface and
 mass transport in solvent-free epoxidation by H2O2 and TBHP: a study with
 organic salts of the [PMo12O40]3&#x2212; anion
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3466
_journal_paper_doi               10.1039/c3nj00523b
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         '(C9 H14 N)3, O40 P Mo12'
_chemical_formula_sum            'C27 H42 Mo12 N3 O40 P'
_chemical_formula_weight         2230.89
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.754(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9672(3)
_cell_length_b                   18.6128(4)
_cell_length_c                   24.1420(5)
_cell_measurement_reflns_used    34138
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.89
_cell_volume                     5340.1(2)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2012)'
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Xcalibur, Sapphire1, long nozzle'
_diffrn_measurement_method       '\w scans'
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            54250
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    2.854
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
CrysAlisPro (Agilent Technologies, 2012)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       box
_exptl_crystal_F_000             4256
_exptl_crystal_size_max          0.447
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.254
_refine_diff_density_max         1.854
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         12008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0153P)^2^+29.0222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                10938
_reflns_number_total             12008
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3nj00523b.txt
_cod_data_source_block           (BP)3PMo12O40
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7053187