C-Trifluoromethyl-Substituted 1,2-Oxaphosphetane Complexes: Synthetic and Structural Study
Kyri, Andreas W.; Schnakenburg, Gregor; Streubel, Rainer; Organometallics 35 (2016) 563–; doi:10.1021/acs.organomet.5b00974

data_4088263
_publ_section_title
;
 C-Trifluoromethyl-Substituted 1,2-Oxaphosphetane Complexes: Synthetic and
 Structural Study
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              563
_journal_paper_doi               10.1021/acs.organomet.5b00974
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C27 H18 F3 O6 P W'
_chemical_formula_sum            'C27 H18 F3 O6 P W'
_chemical_formula_weight         710.23
_chemical_name_systematic        AKY-487
_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     iterative
_audit_creation_date             2015-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.09 svn.r3130 for OlexSys, GUI svn.r4987)
;
_cell_angle_alpha                71.032(3)
_cell_angle_beta                 76.087(3)
_cell_angle_gamma                75.469(4)
_cell_formula_units_Z            2
_cell_length_a                   9.6002(10)
_cell_length_b                   10.5444(11)
_cell_length_c                   13.8429(14)
_cell_measurement_reflns_used    8571
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.75
_cell_volume                     1263.3(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_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  0.0286
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12605
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.079
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.699
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5035
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1344 before and 0.0407 after correction.
The Ratio of minimum to maximum transmission is 0.6749.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.165
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         4756
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0237
_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^)+(0.0104P)^2^+2.0735P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4281
_reflns_number_total             4756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00974_si_001.cif
_cod_data_source_block           3940f
_cod_database_code               4088263
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
2. Shared sites
{F1, F1'}
{F2, F2'}
3. Restrained distances
 C3'-F3'
 1.39 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(F3') \\sim Ueq, Uanis(C3') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F1) = Uanis(F1')
Uanis(F2) = Uanis(F2')
5. Others
 Sof(C1')=Sof(H1')=Sof(C3')=Sof(F1')=Sof(F2')=Sof(F3')=Sof(H2BC)=Sof(H2BD)=1-
 FVAR(1)
 Sof(C1)=Sof(H1)=Sof(C3)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(H2AA)=Sof(H2AB)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C1'(H1')
6.b Secondary CH2 refined with riding coordinates:
 C2(H2AA,H2AB), C2(H2BC,H2BD)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
;
_shelx_res_checksum              9889
_shelx_hkl_checksum              73103
_olex2_submission_special_instructions 'No special instructions were received'