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_7714987
_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         'C48 H74 O P2'
_chemical_formula_sum            'C48 H74 O P2'
_chemical_formula_weight         729.01
_chemical_melting_point          521.0(10)
_chemical_name_common            (EMind)(O=)P=P(EMind)
_chemical_name_systematic        'EMind 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   difmap
_atom_sites_solution_primary     'dual space'
_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                93.270(3)
_cell_angle_beta                 90.315(3)
_cell_angle_gamma                102.939(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7135(4)
_cell_length_b                   11.7140(4)
_cell_length_c                   17.7296(6)
_cell_measurement_reflns_used    11145
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.3400
_cell_measurement_theta_min      1.8070
_cell_volume                     2164.62(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    SHELXT-2018/2
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            102503
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.194
_diffrn_reflns_theta_min         1.951
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene-d6'
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         11259
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0403P)^2^+2.1609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1532
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7332
_reflns_number_total             11259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04348g2.cif
_cod_data_source_block           EMindP2O
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '520-522' was changed to
'521.0(10)' -- the average value was taken and precision was
estimated.

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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

 Adding full bibliography for 7714986--7714987.cif.
;
_cod_database_code               7714987
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.969
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              50044