Hydrogen peroxide adducts of triarylphosphine oxides.
Arp, Fabian F.; Bhuvanesh, Nattamai; Blümel, Janet; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14312–14325; doi:10.1039/c9dt03070k

data_7701780
_publ_section_title
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 Hydrogen peroxide adducts of triarylphosphine oxides.
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_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14312
_journal_page_last               14325
_journal_paper_doi               10.1039/c9dt03070k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C20 H19 O P, H2 O2'
_chemical_formula_sum            'C20 H21 O3 P'
_chemical_formula_weight         340.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2019-02-20 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.431(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9873(5)
_cell_length_b                   15.7070(7)
_cell_length_c                   12.4419(6)
_cell_measurement_reflns_used    9729
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.577
_cell_measurement_theta_min      2.594
_cell_volume                     1727.32(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            68772
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.628
_diffrn_reflns_theta_min         2.110
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.7411
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1232 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.9386.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.133
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4000
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+1.8142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3096
_reflns_number_total             4000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03070k2.cif
_cod_data_source_block           ffe010
_cod_database_code               7701780
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
O2 \\sim O3 \\sim O2A \\sim O3A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 O2, O3, O2A, O3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O2A)=Sof(H2A)=Sof(O3A)=Sof(H3AA)=1-FVAR(1)
 Sof(O2)=Sof(H2)=Sof(O3)=Sof(H3A)=FVAR(1)
5.a Riding coordinates:
 O2(H2), O3(H3A), O2A(H2A), O3A(H3AA)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C18(H18), C19(H19)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              14348
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'