Another side of the oxazaphospholidine oxide chiral ortho-directing group
Martins, Nelson; Mateus, Nuno; Vinci, Daniele; Saidi, Ourida; Brigas, Amadeu; Bacsa, John; Xiao, Jianliang; Organic & Biomolecular Chemistry 10 (2012) 4036–; doi:10.1039/c2ob25187f

data_7152328
_publ_section_title
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 Another side of the oxazaphospholidine oxide chiral ortho-directing group
;
_journal_issue                   20
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              4036
_journal_paper_doi               10.1039/c2ob25187f
_journal_volume                  10
_journal_year                    2012
_chemical_absolute_configuration rmad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C20 H22 Fe N O2 P'
_chemical_formula_sum            'C20 H22 Fe N O2 P'
_chemical_formula_weight         395.21
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.8170(3)
_cell_length_b                   12.8442(7)
_cell_length_c                   23.6728(13)
_cell_measurement_reflns_used    7902
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.2
_cell_measurement_theta_min      2.6
_cell_volume                     1768.71(16)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.24 beta (release 23.09.2004 CrysAlis171 .NET)
(compiled Sep 23 2004,08:58:26)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.24 beta (release 23.09.2004 CrysAlis171 .NET)
(compiled Sep 23 2004,08:58:26)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.24 beta (release 23.09.2004 CrysAlis171 .NET)
(compiled Sep 23 2004,08:58:26)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
1 omega -54.00 61.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 30.0000 -79.0000 0.0000 0.0000 0.0000 115

2 omega -54.00 61.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 30.0000 -79.0000 90.0000 0.0000 0.0000 115

3 omega -54.00 61.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 30.0000 -79.0000 180.0000 0.0000 0.0000 115

4 omega -54.00 61.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 30.0000 -79.0000 270.0000 0.0000 0.0000 115

;
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       '\w and \f'
_diffrn_orient_matrix_UB_11      0.0036964142
_diffrn_orient_matrix_UB_12      0.0330105662
_diffrn_orient_matrix_UB_13      -0.0239885337
_diffrn_orient_matrix_UB_21      0.1095074508
_diffrn_orient_matrix_UB_22      -0.0202630069
_diffrn_orient_matrix_UB_23      -0.0072179419
_diffrn_orient_matrix_UB_31      -0.0535067056
_diffrn_orient_matrix_UB_32      -0.0393614603
_diffrn_orient_matrix_UB_33      -0.0164380486
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            17933
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.29
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.5739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         5386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0726
_reflns_number_gt                4949
_reflns_number_total             5386
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2ob25187f.txt
_cod_data_source_block           lnm42
_cod_database_code               7152328