Unexpected synthesis of (bis(diphenylphosphinoyl)ethane)·2(2,2-dihydroperoxypropane) 1∶2 adduct: a new route to stable organic dihydroperoxides
Pettinari, Claudio; Marchetti, Fabio; Cingolani, Augusto; Drozdov, Andrei; Troyanov, Sergei; Chemical Communications  (2000) 1901–; doi:10.1039/b005221n

data_7111045
_publ_section_title
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 Unexpected synthesis of
 (bis(diphenylphosphinoyl)ethane)&#x00B7;2(2,2-dihydroperoxypropane)
 1&#x2236;2 adduct: a new route to stable organic dihydroperoxides
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_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              1901
_journal_paper_doi               10.1039/b005221n
_journal_year                    2000
_chemical_formula_sum            'C32 H40 O10 P2'
_chemical_formula_weight         646.58
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.447(3)
_cell_length_b                   10.989(2)
_cell_length_c                   19.907(4)
_cell_measurement_reflns_used    904
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      5
_cell_volume                     3379.2(11)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device       IPDS(Stoe)
_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  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       19
_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       -25
_diffrn_reflns_number            11022
_diffrn_reflns_theta_max         26.90
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.0012(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.934
_refine_ls_goodness_of_fit_obs   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_restrained_S_obs      1.044
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_obs          0.0362
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0940
_refine_ls_wR_factor_obs         0.0821
_reflns_number_observed          2081
_reflns_number_total             3414
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b005221nsup1.cif
_cod_data_source_block           peroxo
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7111045