An approach to 7-aza-1-phosphanorbornane complexes: strain promoted rearrangement of 1-iminylphosphirane complexes and cycloaddition with olefins.
Xu, Yang; Wang, Min; Wei, Donghui; Tian, Rongqiang; Duan, Zheng; Mathey, François; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5523–5526; doi:10.1039/c9dt00838a

data_7049588
_publ_section_title
;
 An approach to 7-aza-1-phosphanorbornane complexes: strain promoted
 rearrangement of 1-iminylphosphirane complexes and cycloaddition with
 olefins.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5523
_journal_page_last               5526
_journal_paper_doi               10.1039/c9dt00838a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C30 H21 N2 O7 P W'
_chemical_formula_sum            'C30 H21 N2 O7 P W'
_chemical_formula_weight         736.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-02
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Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
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_audit_update_record
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2019-01-23 deposited with the CCDC.    2019-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.372(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.786(3)
_cell_length_b                   9.1802(5)
_cell_length_c                   19.895(2)
_cell_measurement_reflns_used    4461
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1150
_cell_measurement_theta_min      3.8850
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -10.00   16.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.1755  -99.0000  -60.0000 26

  2 omega    3.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0661   57.0000  -60.0000 80

  3 omega  -48.00   72.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0661    0.0000  -90.0000 120
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      -0.0415423000
_diffrn_orient_matrix_UB_12      0.0311742000
_diffrn_orient_matrix_UB_13      -0.0118664000
_diffrn_orient_matrix_UB_21      0.0006152000
_diffrn_orient_matrix_UB_22      -0.0027799000
_diffrn_orient_matrix_UB_23      0.0358562000
_diffrn_orient_matrix_UB_31      0.0183395000
_diffrn_orient_matrix_UB_32      0.0706689000
_diffrn_orient_matrix_UB_33      0.0066107000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12646
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.362
_diffrn_reflns_theta_min         3.423
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.152
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.726
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0451
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+2.9439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4533
_reflns_number_total             5815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00838a2.cif
_cod_data_source_block           201706100
_cod_depositor_comments
'Adding full bibliography for 7049588--7049591.cif.'
_cod_original_cell_volume        2855.0(8)
_cod_database_code               7049588
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C38H70N2O2W1
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
;
_olex2_submission_special_instructions 'No special instructions were received'