CPh3 as a functional group in P-heterocyclic chemistry: elimination of HCPh3 in the reaction of P-CPh3 substituted Li/Cl phosphinidenoid complexes with Ph2C[double bond, length as m-dash]O.
García, C Murcia; Ferao, A. Espinosa; Schnakenburg, G.; Streubel, R.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2378–2385; doi:10.1039/c5dt04595a

data_7037937
_publ_section_title
;
 CPh3 as a functional group in P-heterocyclic chemistry: elimination of
 HCPh3 in the reaction of P-CPh3 substituted Li/Cl phosphinidenoid
 complexes with Ph2C[double bond, length as m-dash]O.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2378
_journal_page_last               2385
_journal_paper_doi               10.1039/c5dt04595a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C37 H25 O6 P W'
_chemical_formula_sum            'C37 H25 O6 P W'
_chemical_formula_weight         780.39
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-09-10 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                98.301(4)
_cell_angle_beta                 94.830(4)
_cell_angle_gamma                112.865(4)
_cell_formula_units_Z            2
_cell_length_a                   9.4174(14)
_cell_length_b                   10.7473(14)
_cell_length_c                   17.631(2)
_cell_measurement_reflns_used    1853
_cell_measurement_temperature    123
_cell_measurement_theta_max      23.95
_cell_measurement_theta_min      2.45
_cell_volume                     1607.6(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0995
_diffrn_reflns_av_unetI/netI     0.1408
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14721
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.73
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.688
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5374
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
Estimated minimum and maximum transmission:  0.5374  0.7460
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.268
_refine_diff_density_min         -1.704
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5711
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0112P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                4003
_reflns_number_total             5711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04595a2.cif
_cod_data_source_block           3425f
_cod_depositor_comments
'Adding full bibliography for 7037934--7037937.cif.'
_cod_database_code               7037937
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C3(H3)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
;