Selective Synthesis and Stabilization of Peroxides via Phosphine Oxides
Arp, Fabian Felix; Ahn, Shin Hye; Bhuvanesh, Nattamai; Bluemel, Janet; New Journal of Chemistry 43 (2019) 17174–17181; doi:10.1039/C9NJ04858H

data_7058905
_publ_section_title
;
 Selective Synthesis and Stabilization of Peroxides via Phosphine Oxides
;
_journal_issue                   44
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17174
_journal_page_last               17181
_journal_paper_doi               10.1039/C9NJ04858H
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C5 H10 O6'
_chemical_formula_sum            'C5 H10 O6'
_chemical_formula_weight         166.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-02-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_audit_update_record
;
2019-10-14 deposited with the CCDC.    2019-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.306(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.5661(6)
_cell_length_b                   15.4167(15)
_cell_length_c                   8.8545(9)
_cell_measurement_reflns_used    2704
_cell_measurement_temperature    100.03
_cell_measurement_theta_max      27.487
_cell_measurement_theta_min      2.643
_cell_volume                     759.20(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX 3 (Bruker-AXS, Madison WI)'
_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      100.03
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 1.000
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2327
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.642
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1043 before and 0.0593 after correction.
 The Ratio of minimum to maximum transmission is 0.75.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0929 before and 0.0600 after correction.
 The Ratio of minimum to maximum transmission is 0.75.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 16324 reflections, Rint = 0.0627
 (9311 with I > 3sig(I), Rint = 0.0544)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0467P)^2^+0.4994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1859
_reflns_number_total             2327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04858h2.cif
_cod_data_source_block           ga229b
_cod_database_code               7058905
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.970
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.605(2) 0.395(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3.a Riding coordinates:
 O4(H4), O6(H6)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              72253
_olex2_submission_special_instructions 'No special instructions were received'