Nonstereospecific 1,3-Dipolar Cycloaddition Reactions of Azomethine Ylides: Proof of the Structures for Four Diastereoisomeric [3+2] Cycloadducts
Breu, Josef; Range, Klaus-Jürgen; Weber, Andreas; Sauer, Jürgen; Acta Crystallographica Section C 54 (1998) 509–513; doi:10.1107/S010827019701439X

data_2007175
_publ_section_title
;
 Nonstereospecific 1,3-Dipolar Cycloaddition Reactions of Azomethine
 Ylides: Proof of the Structures for Four Diastereoisomeric [3+2]
 Cycloadducts
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              509
_journal_page_last               513
_journal_paper_doi               10.1107/S010827019701439X
_journal_volume                  54
_journal_year                    1998
_chemical_formula_sum            'C34 H39 N5'
_chemical_formula_weight         517.72
_chemical_name_systematic
;
1,1-Dimethyl-4a-pyrolidin-1-yl-2,8b-di-p-tolyl-1,1a,4a,5,6,7,8,8a,8b,8c-
decahydro-cis-1a-cis-4a-transoid-8a,8b-transoid-8b,8c-3,3a-diaza-cyclopropa
[c]fluoren-4,4-dicarbonitril
;
_space_group_IT_number           14
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_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
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_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2212(4)
_cell_length_b                   18.0246(10)
_cell_length_c                   17.4099(8)
_cell_measurement_reflns_used    4615
_cell_measurement_temperature    170
_cell_measurement_theta_max      24.75
_cell_measurement_theta_min      2.38
_cell_volume                     2840.4(2)
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution
'SIR92 (Altomare, Cascarano, Giacovazzo & Guagliardi, 1993)'
_diffrn_ambient_temperature      170
_diffrn_measurement_device       'STOE IPDS'
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_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
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_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_max         24.81
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.07
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_meas      ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.139
_refine_diff_density_min         -0.111
_refine_ls_extinction_method     none
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_refine_ls_restrained_S_obs      0.950
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_refine_ls_R_factor_obs          .0344
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_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0141P)^2^]  where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0551
_refine_ls_wR_factor_obs         .0503
_reflns_number_observed          2319
_reflns_number_total             4535
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            jz1241.cif
_cod_data_source_block           VII
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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^)+(0.0141P)^2^] 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^)+(0.0141P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        ' C34 H39 N5'
_cod_database_code               2007175