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_4088265
_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         'C16 H21 F6 O6 P Si2 W'
_chemical_formula_sum            'C16 H21 F6 O6 P Si2 W'
_chemical_formula_weight         694.33
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                70.869(5)
_cell_angle_beta                 79.168(6)
_cell_angle_gamma                66.889(5)
_cell_formula_units_Z            2
_cell_length_a                   8.9748(9)
_cell_length_b                   10.3623(9)
_cell_length_c                   15.4170(13)
_cell_measurement_reflns_used    4087
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.47
_cell_volume                     1243.0(2)
_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
;
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 0.984
_diffrn_measured_fraction_theta_max 0.981
_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  0.0426
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12106
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.76
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.880
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5698
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0857 before and 0.0476 after correction.
The Ratio of minimum to maximum transmission is 0.7638.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.431
_refine_diff_density_min         -2.734
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         5889
_refine_ls_number_restraints     293
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+5.5276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                4355
_reflns_number_total             5889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00974_si_001.cif
_cod_data_source_block           3684f
_cod_database_code               4088265
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si2-C10S = Si2-C10T = Si2-C9S = Si2-C9T = Si2-C11S = Si2-C11T
 1.81 with sigma of 0.001
 Si1-C6S = Si1-C7S = Si1-C8S
 1.81 with sigma of 0.001
 F2A-F3A
 2.2 with sigma of 0.01
 C3-F3A
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C11 \\sim C9 \\sim C10 \\sim C11S \\sim C9S \\sim C10S \\sim C11T \\sim C9T
\\sim C10T: within 1.7A with sigma of 0.007 and sigma for terminal atoms of
0.014
C6 \\sim C7 \\sim C8 \\sim C6S \\sim C7S \\sim C8S: within 1.7A with sigma of
0.007 and sigma for terminal atoms of 0.014
F1 \\sim F2 \\sim F3 \\sim F1A \\sim F2A \\sim F3A \\sim C3: within 1.7A with
sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(C13) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C12S) \\sim Ueq,
Uanis(C14S) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F4A) \\sim
Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2)
\\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2A) \\sim Ueq,
Uanis(F3A) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(O3S) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(O1) = Uanis(C1S)
Uanis(O1S) = Uanis(C1)
4. Others
 Sof(C6S)=Sof(H6SA)=Sof(H6SB)=Sof(H6SC)=Sof(C7S)=Sof(H7SA)=Sof(H7SB)=Sof(H7SC)=
 Sof(C8S)=Sof(H8SA)=Sof(H8SB)=Sof(H8SC)=1-FVAR(1)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(1)
 Sof(C12S)=Sof(C14S)=Sof(O5S)=Sof(O3S)=1-FVAR(2)
 Sof(O3)=Sof(O5)=Sof(C14)=Sof(C12)=FVAR(2)
 Sof(O1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=1-FVAR(3)
 Sof(O1)=Sof(C1)=Sof(H1A)=Sof(H1B)=FVAR(3)
 Sof(F6A)=Sof(F4A)=Sof(F5A)=1-FVAR(4)
 Sof(F6)=Sof(F4)=Sof(F5)=FVAR(4)
 Sof(F2A)=Sof(F3A)=Sof(F1A)=1-FVAR(5)
 Sof(F1)=Sof(F3)=Sof(F2)=FVAR(5)
 Fixed Sof: C9(0.3) H9A(0.3) H9B(0.3) H9C(0.3) C10(0.3) H10A(0.3) H10B(0.3)
 H10C(0.3) C11(0.3) H11A(0.3) H11B(0.3) H11C(0.3) C11S(0.43) H11D(0.43)
 H11E(0.43) H11F(0.43) C9S(0.43) H9SA(0.43) H9SB(0.43) H9SC(0.43) C10S(0.43)
 H10D(0.43) H10E(0.43) H10F(0.43) C9T(0.27) H9TA(0.27) H9TB(0.27) H9TC(0.27)
 C10T(0.27) H10G(0.27) H10H(0.27) H10I(0.27) C11T(0.27) H11G(0.27) H11H(0.27)
 H11I(0.27)
5.a Ternary CH refined with riding coordinates:
 C5(H5)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1S(H1SA,H1SB)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C11S(H11D,H11E,
 H11F), C9S(H9SA,H9SB,H9SC), C10S(H10D,H10E,H10F), C9T(H9TA,H9TB,H9TC),
 C10T(H10G,H10H,H10I), C11T(H11G,H11H,H11I), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C),
 C8(H8A,H8B,H8C), C6S(H6SA,H6SB,H6SC), C7S(H7SA,H7SB,H7SC), C8S(H8SA,H8SB,H8SC)
;
_olex2_submission_special_instructions 'No special instructions were received'