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_7701779
_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         '1(C19 H17 O P), 0.5(H2 O2)'
_chemical_formula_sum            'C19 H18 O2 P'
_chemical_formula_weight         309.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-28
_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                94.697(5)
_cell_angle_beta                 90.536(5)
_cell_angle_gamma                102.113(5)
_cell_formula_units_Z            4
_cell_length_a                   8.606(3)
_cell_length_b                   10.259(3)
_cell_length_c                   18.844(6)
_cell_measurement_reflns_used    9217
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.613
_cell_measurement_theta_min      2.225
_cell_volume                     1620.6(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      110.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_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  0.0286
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34408
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.613
_diffrn_reflns_theta_min         1.085
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1368 before and 0.0442 after correction.
The Ratio of minimum to maximum transmission is 0.8995.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.526
_exptl_crystal_size_mid          0.481
_exptl_crystal_size_min          0.226
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         7421
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.268
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+2.8388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6449
_reflns_number_total             7421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03070k2.cif
_cod_data_source_block           fe011
_cod_original_cell_volume        1620.7(9)
_cod_database_code               7701779
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.914
_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. Restrained distances
 O4-O3 \\sim O4A-O3A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O3 \\sim H3A \\sim O4 \\sim H4A \\sim O4A \\sim O3A: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C7) = Uanis(C7A)
4. Rigid body (RIGU) restrains
 O3, H3A, O4, H4A, O4A, O3A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Others
 Sof(H19)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=1-FVAR(1)
 Sof(H2)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(1)
 Sof(O3A)=Sof(H3AA)=Sof(O4A)=Sof(H4AA)=1-FVAR(2)
 Sof(O3)=Sof(H3A)=Sof(O4)=Sof(H4A)=FVAR(2)
6.a Riding coordinates:
 C2(H2), C19(H19), O3(H3A), O4(H4A), O3A(H3AA), O4A(H4AA)
6.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC)
6.c 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), C15(H15), C16(H16), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24),
  C25(H25), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34),
 C35(H35), C36(H36), C37(H37), C38(H38)
6.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C)
;
_shelx_res_checksum              80895
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'