A novel route to C-unsubstituted 1,2-oxaphosphetane and 1,2-oxaphospholane complexes.
Kyri, A. W.; Schnakenburg, G.; Streubel, R.; Chemical communications (Cambridge, England) 52 (2016) 8593–8595; doi:10.1039/c6cc04667c

data_7124797
_publ_section_title
;
 A novel route to C-unsubstituted 1,2-oxaphosphetane and
 1,2-oxaphospholane complexes.
;
_journal_issue                   55
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8593
_journal_page_last               8595
_journal_paper_doi               10.1039/c6cc04667c
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C14 H24 I O6 P Si2 W'
_chemical_formula_sum            'C14 H24 I O6 P Si2 W'
_chemical_formula_weight         686.23
_chemical_name_systematic        AKY-424
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2016-03-24 deposited with the CCDC.
2016-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                86.293(10)
_cell_angle_beta                 81.810(10)
_cell_angle_gamma                65.584(9)
_cell_formula_units_Z            2
_cell_length_a                   9.179(3)
_cell_length_b                   10.433(4)
_cell_length_c                   14.066(5)
_cell_measurement_reflns_used    5405
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      2.59
_cell_volume                     1214.0(8)
_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      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.852
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8231
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.46
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.216
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.3610
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1401 before and 0.0797 after correction.
The Ratio of minimum to maximum transmission is 0.4840.
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    1.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.694
_refine_diff_density_min         -4.762
_refine_diff_density_rms         0.431
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3734
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.1918
_refine_ls_R_factor_gt           0.1405
_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^)+(0.0001P)^2^+196.1710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3049
_refine_ls_wR_factor_ref         0.3359
_reflns_number_gt                2777
_reflns_number_total             3734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc04667c2.cif
_cod_data_source_block           3760f
_cod_original_cell_volume        1214.0(7)
_cod_database_code               7124797
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H
 2.4 with sigma of 0.01
 P-H
 1.43 with sigma of 0.01
3. Rigid bond restraints
 Si1, C4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq:
with sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(O6) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
5.a Ternary CH refined with riding coordinates:
 C3(H3)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C5(H5A,
 H5B,H5C), C7(H7A,H7B,H7C)
;
_olex2_submission_special_instructions 'No special instructions were received'