(<i>Z</i>)-<i>N</i>-[(2<i>R</i>,3<i>R</i>)-2-(<i>tert</i>-Butoxycarbonylamino)-3-(<i>tert</i>-butyldiphenylsiloxy)butylidene]benzylamine <i>N</i>-Oxide
Merino, P.; Merchan, F. L.; Tejero, T.; Lanaspa, A.; Acta Crystallographica Section C 51 (1995) 1949–1950; doi:10.1107/S0108270195004343

data_2003936
_publ_section_title
;(<i>Z</i>)-<i>N</i>-[(2<i>R</i>,3<i>R</i>)-2-(<i>tert</i>-Butoxycarbonylamino)-3-(<i>tert</i>-butyldiphenylsiloxy)butylidene]benzylamine
 <i>N</i>-Oxide
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1949
_journal_page_last               1950
_journal_paper_doi               10.1107/S0108270195004343
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source        'chemical synthesis'
_chemical_formula_sum            'C32 H42 N2 O4 Si'
_chemical_formula_weight         546.77
_chemical_melting_point          400
_chemical_name_systematic
;
 (Z)-N-[(2R,3R)-2-(tert-Butoxycarbonylamino)-3-(tert-
butyldiphenylsilyloxy)butylidene]benzylamine N-oxide
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.002(2)
_cell_length_b                   14.274(3)
_cell_length_c                   21.976(4)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.847
_cell_measurement_theta_min      9.449
_cell_volume                     3137.5(11)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1992)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXL93
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'Profile data from 2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0978
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3015
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        7.26
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type
;semi-empirical (ellipsoidal) refined from \y scan (North, Philips & Mathews,
1968)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.176
_refine_ls_abs_structure_Flack   -0.22(40)
_refine_ls_extinction_coef       0.0047(12)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.078
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_hydrogen_treatment
;
H atoms refined as riding model (except for H1)
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         2824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_restrained_S_obs      1.132
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_obs          0.0568
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0580P)^2^ + 0.7204P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1593
_refine_ls_wR_factor_obs         0.1148
_reflns_number_observed          1648
_reflns_number_total             2827
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            na1167.cif
_cod_data_source_block           nitro1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'YES' changed to 'yes' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (8
times).

'_geom_angle_publ_flag' value 'YES' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (8
times).

'_geom_torsion_publ_flag' value 'YES' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (2
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2003936