(2a<i>S</i>,3<i>S</i>,6<i>S</i>,7<i>S</i>,7b<i>R</i>)-7-[(Dimethylphenyl)silyl]-2-oxo-6-[(1<i>R</i>,2<i>S</i>)-2-phenylcyclohexyloxy]-2a,3,6,7,7a,7b-hexahydro-2<i>H</i>-1,4,5-trioxa-4a-azacyclopenta[<i>cd</i>]indene-3-carboxylic Acid 1-Methylethyl Ester
Thorarensen, A.; Swiss, K. A.; Denmark, S. E.; Acta Crystallographica Section C 52 (1996) 2558–2561; doi:10.1107/S0108270196005434

data_2005548
_publ_section_title
;(2a<i>S</i>,3<i>S</i>,6<i>S</i>,7<i>S</i>,7b<i>R</i>)-7-[(Dimethylphenyl)silyl]-2-oxo-6-[(1<i>R</i>,2<i>S</i>)-2-phenylcyclohexyloxy]-2a,3,6,7,7a,7b-hexahydro-2<i>H</i>-1,4,5-trioxa-4a-azacyclopenta[<i>cd</i>]indene-3-carboxylic
 Acid 1-Methylethyl Ester
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2558
_journal_page_last               2561
_journal_paper_doi               10.1107/S0108270196005434
_journal_volume                  52
_journal_year                    1996
_chemical_formula_analytical     'C31 H39 N1 O7 Si1'
_chemical_formula_moiety         'C31 H39 N1 O7 Si1'
_chemical_formula_structural     'C31 H39 N1 O7 Si1'
_chemical_formula_sum            'C31 H39 N O7 Si'
_chemical_formula_weight         565.72
_chemical_name_systematic
;
(2aS,3S,6S,7S,7bR)-2-oxo-6-[(1R,2S)-2-phenylcyclohexyloxy]-8-
[(dimethylphenyl)silyl]-2a,3,6,7,7a,7b-hexahydro-2H-1,4,5-trioxa-4a-
azacyclopenta[cd]indene-3-carboxylic Acid 1-Methylethyl Ester
;
_chemical_temperature_decomposition 210
_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                   9.9730(10)
_cell_length_b                   10.7410(10)
_cell_length_c                   27.527(3)
_cell_measurement_reflns_used    270
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      1.48
_cell_volume                     2948.7(5)
_computing_cell_refinement       'SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'SHELXTL-Plus (Siemens, 1994) and ORTEP (Johnson, 1971)'
_computing_publication_material  'CIFTAB SHELXL93'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measurement_device       'Siemens 3-circle platform CCD'
_diffrn_measurement_method       '\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  0.1862
_diffrn_reflns_av_sigmaI/netI    0.1890
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            12795
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count '63 frames'
_diffrn_standards_interval_time  390
_diffrn_standards_number         24
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'hollow rod'
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.282
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.8(4)
_refine_ls_extinction_coef       0.0020(4)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.116
_refine_ls_goodness_of_fit_obs   1.236
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         4008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_restrained_S_obs      1.236
_refine_ls_R_factor_all          0.1905
_refine_ls_R_factor_obs          0.0905
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+5.5747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1653
_refine_ls_wR_factor_obs         0.1245
_reflns_number_observed          2265
_reflns_number_total             4088
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sk1015.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '210
dec.'. The value '210 dec.' was changed to '210'.

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

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:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+5.5747P] where P=(Fo^2^+2Fc^2^)/3' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+5.5747P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C31 H39 N1 O7 Si1'
_cod_database_code               2005548