Ring opening of a sterically crowded 1,2-oxaphosphetane complex.
Kyri, A. W.; Brehm, P.; Schnakenburg, G.; Streubel, R.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2904–2909; doi:10.1039/c7dt00136c

data_7042060
_publ_section_title
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 Ring opening of a sterically crowded 1,2-oxaphosphetane complex.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2904
_journal_page_last               2909
_journal_paper_doi               10.1039/c7dt00136c
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C36 H34 F6 Li O11 P W, 0.5(C4 H10 O)'
_chemical_formula_sum            'C38 H39 F6 Li O11.5 P W'
_chemical_formula_weight         1015.45
_chemical_name_systematic        AKY-488-2
_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
_audit_creation_date             2017-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2017-01-10 deposited with the CCDC.
2017-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                86.722(3)
_cell_angle_beta                 74.872(2)
_cell_angle_gamma                73.209(3)
_cell_formula_units_Z            4
_cell_length_a                   11.7408(5)
_cell_length_b                   18.5934(8)
_cell_length_c                   20.0735(8)
_cell_measurement_reflns_used    9524
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.31
_cell_measurement_theta_min      2.29
_cell_volume                     4049.1(3)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0858
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            105146
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.468
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.979
_exptl_absorpt_correction_T_max  0.5865
_exptl_absorpt_correction_T_min  0.4057
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.1147 before and 0.0646 after correction. The Ratio 
of minimum to maximum transmission is 0.6917. 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    1.666
_exptl_crystal_description       plate
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.023
_refine_diff_density_min         -1.908
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1058
_refine_ls_number_reflns         19509
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0674P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12783
_reflns_number_total             19509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00136c1.cif
_cod_data_source_block           4012f
_cod_depositor_comments
;
Adding full bibliography for 7042059--7042062.cif.

2017-11-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C76 H78 F12 Li2 O23 P2 W2'
_cod_original_formula_weight         2030.90
_cod_original_formula_moiety         '2(C36 H34 F6 Li O11 P W), C4 H10 O'
_cod_original_formula_units_Z            2
_cod_database_code               7042060
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.755
_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, All O(H) groups
2. Restrained distances
 O12-C39
 1.49 with sigma of 0.01
3. Rigid bond restraints
 F5, C4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F1', C3'
 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(C40) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C18) \\sim Ueq, Uanis(C3') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1'(H1'A,H1'B), C29(H29A,H29B), C28(H28A,H28B), C31(H31A,H31B),
 C26(H26A,H26B), C30(H30A,H30B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B),
  C38(H38A,H38B), C39(H39A,H39B), C24'(H24C,H24D), C30'(H30C,H30D), C29'(H29C,
 H29D), C25'(H25C,H25D), C31'(H31C,H31D), C26'(H26C,H26D), C27'(H27C,H27D),
 C28'(H28C,H28D)
5.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C7(H7), C14(H14), C11(H11), C23(H23), C11'(H11'), C17(H17),
 C16'(H16'), C23'(H23'), C20'(H20'), C7'(H7'), C15(H15), C10(H10), C9'(H9'),
 C8'(H8'), C17'(H17'), C22(H22), C13(H13), C14'(H14'), C21(H21), C19(H19),
 C16(H16), C8(H8), C15'(H15'), C22'(H22'), C9(H9), C19'(H19'), C21'(H21'),
 C10'(H10'), C13'(H13')
5.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C40(H40A,H40B,H40C)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O1'(H1')
;
_olex2_submission_special_instructions 'No special instructions were received'