Selective monooxygenation of diphosphenes with molecular oxygen.
Kawase, Yuria; Tsujimoto, Shota; Obayashi, Tomohiro; Kimura, Satoshi; Ito, Kanta; Ikoma, Shotaro; Ota, Kei; Hashizume, Daisuke; Matsuo, Tsukasa; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1956–1960; doi:10.1039/d3dt04348g

data_7714986
_publ_section_title
;
 Selective monooxygenation of diphosphenes with molecular oxygen.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1956
_journal_page_last               1960
_journal_paper_doi               10.1039/d3dt04348g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C56 H90 O P2'
_chemical_formula_sum            'C56 H90 O P2'
_chemical_formula_weight         841.21
_chemical_melting_point          498.0(10)
_chemical_name_common            (Eind)(O=)P=P(Eind)
_chemical_name_systematic        'Eind diphosphene oxide'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2023-11-25 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                89.981(9)
_cell_angle_beta                 85.861(8)
_cell_angle_gamma                68.598(7)
_cell_formula_units_Z            1
_cell_length_a                   8.117(2)
_cell_length_b                   10.258(3)
_cell_length_c                   15.819(5)
_cell_measurement_reflns_used    3556
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.18
_cell_measurement_theta_min      2.46
_cell_volume                     1222.7(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23732
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.415
_diffrn_reflns_theta_min         2.525
_diffrn_source                   'normal-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         7304
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0636P)^2^+0.1794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5214
_reflns_number_total             7304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04348g2.cif
_cod_data_source_block           EindP-P-O
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '497-499' was changed to
'498.0(10)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7714986--7714987.cif.
;
_cod_original_cell_volume        1222.6(6)
_cod_database_code               7714986
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.983
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              53829