Effects of diminished steric protection at phosphorus on stability and reactivity of oxaphosphirane complexes.
Fassbender, J.; Schnakenburg, G.; Espinosa Ferao, A.; Streubel, R.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9347–9354; doi:10.1039/c8dt01979g

data_7046904
_publ_section_title
;
 Effects of diminished steric protection at phosphorus on stability and
 reactivity of oxaphosphirane complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9347
_journal_page_last               9354
_journal_paper_doi               10.1039/c8dt01979g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C19 H21 O6 P W'
_chemical_formula_sum            'C19 H21 O6 P W'
_chemical_formula_weight         560.18
_chemical_name_systematic        JF-152
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-03-24 deposited with the CCDC.
2018-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                87.4885(19)
_cell_angle_beta                 74.0260(19)
_cell_angle_gamma                68.0590(16)
_cell_formula_units_Z            2
_cell_length_a                   9.9897(4)
_cell_length_b                   10.2207(4)
_cell_length_c                   11.3156(3)
_cell_measurement_reflns_used    3684
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_cell_volume                     1028.02(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3852
_diffrn_reflns_av_unetI/netI     0.1889
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12583
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.993
_diffrn_reflns_theta_min         2.289
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    5.727
_exptl_absorpt_correction_T_max  0.6211
_exptl_absorpt_correction_T_min  0.3541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_description       plate
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         5.408
_refine_diff_density_min         -6.307
_refine_diff_density_rms         0.448
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4962
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1255P)^2^+4.0396P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2054
_refine_ls_wR_factor_ref         0.2206
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3840
_reflns_number_total             4962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01979g2.cif
_cod_data_source_block           4189
_cod_depositor_comments
'Adding full bibliography for 7046902--7046905.cif.'
_cod_original_cell_volume        1028.02(6)
_cod_database_code               7046904
_shelxl_version_number           2013-2
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C2) \\sim Ueq: with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C9) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.08 and
sigma for terminal atoms of 0.16
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(C16) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              5566
_olex2_submission_special_instructions 'No special instructions were received'