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_7042061
_publ_section_title
;
 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         'C28 H17 F6 O6 P W'
_chemical_formula_sum            'C28 H17 F6 O6 P W'
_chemical_formula_weight         778.23
_chemical_name_systematic        PB-13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.21 svn.r3230 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-01-10 deposited with the CCDC.
2017-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.6203(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.5390(8)
_cell_length_b                   11.5901(6)
_cell_length_c                   32.8290(18)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      2.26
_cell_volume                     5437.2(5)
_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      150.0
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1371
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            106615
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         2.150
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.391
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4359
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1598 before and 0.0810 after correction.
The Ratio of minimum to maximum transmission is 0.5844.
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    1.901
_exptl_crystal_description       plate
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.025
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         13119
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0168P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9555
_reflns_number_total             13119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00136c1.cif
_cod_data_source_block           4641f
_cod_depositor_comments
'Adding full bibliography for 7042059--7042062.cif.'
_cod_database_code               7042061
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.578
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 P1', O1'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2'(H2'A,H2'B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C7'(H7'),
  C8'(H8'), C9'(H9'), C10'(H10'), C11'(H11'), C13'(H13'), C14'(H14'),
 C15'(H15'), C16'(H16'), C17'(H17'), C19'(H19'), C20'(H20'), C21'(H21'),
 C22'(H22'), C23'(H23')
;
_shelx_res_checksum              45195
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'