Construction of Azaspirocyclic Ketones through α-Hydroxyiminium Ion or α-Siloxy Epoxide Semipinacol Rearrangements
Fenster, Michaël D. B.; Patrick, Brian O.; Dake, Gregory R.; Organic Letters 3 (2001) 2109–; doi:10.1021/ol0160708

data_1507517
_publ_section_title
;
 Construction of Azaspirocyclic Ketones through \a-Hydroxyiminium Ion or
 \a-Siloxy Epoxide Semipinacol Rearrangements
;
_journal_issue                   13
_journal_name_full               'Organic Letters'
_journal_page_first              2109
_journal_paper_doi               10.1021/ol0160708
_journal_volume                  3
_journal_year                    2001
_chemical_formula_moiety         'C23 H37 N O5 S Si '
_chemical_formula_sum            'C23 H37 N O5 S Si'
_chemical_formula_weight         467.69
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_date             2000-11-30
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
?
;
_cell_angle_alpha                90
_cell_angle_beta                 102.031(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6837(4)
_cell_length_b                   6.2994(3)
_cell_length_c                   18.8641(8)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    198.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     1241.68(9)
_computing_cell_refinement       'd*TREK (MSC, 1996-1998)'
_computing_data_collection       'd*TREK (MSC, 1996-1998)'
_computing_data_reduction        'd*TREK (MSC, 1996-1998)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SIR97 (Altomare, et. al. 1998)
;
_diffrn_ambient_temperature      198.2
_diffrn_detector_area_resol_mean 11.76
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.03663
_diffrn_reflns_av_sigmaI/netI    0.070
_diffrn_reflns_limit_h_max       15
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_diffrn_reflns_limit_k_min       -8
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_diffrn_reflns_limit_l_min       -25
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_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        0.00
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_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.211
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_exptl_crystal_density_meas      ?
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_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.030
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0520
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo^2^)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0814
_refine_ls_wR_factor_ref         0.039
_reflns_number_gt                4698
_reflns_number_total             5231
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ol0160708_s2.cif
_cod_data_source_block           gd001/MF-G-34-a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:
data name '_geom_bond_atom_site_label_D' replaced with
'_geom_hbond_atom_site_label_D' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_bond_atom_site_label_H' replaced with
'_geom_hbond_atom_site_label_H' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_atom_site_label_a' replaced with
'_geom_hbond_atom_site_label_A' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_bond_distance_DH' replaced with '_geom_hbond_distance_DH'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_distance_HA' replaced with
'_geom_hbond_distance_HA' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_distance_DA' replaced with
'_geom_hbond_distance_DA' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_angle_DHA' replaced with '_geom_hbond_angle_DHA' as
specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_site_symmetry_A' replaced with
'_geom_hbond_site_symmetry_A' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 5005 2017-03-03 11:38:54Z antanas 
;
_cod_original_cell_volume        1241.69(8)
_cod_original_sg_symbol_H-M      'P 21       '
_cod_original_formula_sum        'C23 H37 N O5 S Si '
_cod_database_code               1507517