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_7042062
_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         'C30 H23 F6 O7 P Si W'
_chemical_formula_sum            'C30 H23 F6 O7 P Si W'
_chemical_formula_weight         852.39
_chemical_name_systematic        PB-35
_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             2016-07-29
_audit_creation_method
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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                87.0836(15)
_cell_angle_beta                 82.7857(15)
_cell_angle_gamma                89.8868(13)
_cell_formula_units_Z            2
_cell_length_a                   8.9870(3)
_cell_length_b                   13.1455(3)
_cell_length_c                   13.3173(2)
_cell_measurement_reflns_used    5798
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_cell_volume                     1558.80(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0446
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20755
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.591
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.877
_exptl_absorpt_correction_T_max  1.071
_exptl_absorpt_correction_T_min  0.5781
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.141
_refine_diff_density_min         -1.740
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         7500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+2.0713P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7053
_reflns_number_total             7500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00136c1.cif
_cod_data_source_block           4737
_cod_depositor_comments
'Adding full bibliography for 7042059--7042062.cif.'
_cod_database_code               7042062
_shelxl_version_number           2013-2
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              42099
_olex2_submission_special_instructions 'No special instructions were received'