Effect of Substitution on the Intramolecular 1,3-Dipolar Cycloaddition of Alkene Tethered Münchnones
Guillaume Bélanger; Myriam April; Étienne Dauphin; Stéphanie Roy; Journal of Organic Chemistry 72 (2007) 1104–1111; doi:10.1021/jo061556t

data_4022603
_publ_section_title
;
 Effect of Substitution on the Intramolecular 1,3-Dipolar
 Cycloaddition of Alkene Tethered M\"unchnones
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1104
_journal_page_last               1111
_journal_paper_doi               10.1021/jo061556t
_journal_volume                  72
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H23 N O'
_chemical_formula_sum            'C16 H23 N O'
_chemical_formula_weight         245.35
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-09-25T16:18:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.0500(10)
_cell_length_b                   20.0500(10)
_cell_length_c                   7.090(2)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      35
_cell_measurement_theta_min      30
_cell_measurement_wavelength     1.54176
_cell_volume                     2850.1(8)
_computing_cell_refinement       difrac
_computing_data_collection       difrac
_computing_data_reduction        nrcvax
_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    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.873
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  cad4
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           cuk\a
_diffrn_radiation_wavelength     1.54176
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2346
_diffrn_reflns_theta_full        69.55
_diffrn_reflns_theta_max         69.55
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  0.9984
_exptl_absorpt_correction_T_min  0.8603
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0000(4)
_refine_ls_extinction_expression fc^*^=kfc[1+0.001xfc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     shelxl
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1763
_refine_ls_R_factor_gt           0.0907
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(fo^2^)+(0.1551p)^2^+0.0000p] where p=(fo^2^+2fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2324
_refine_ls_wR_factor_ref         0.2793
_reflns_number_gt                1089
_reflns_number_total             2346
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            jo061556tsi20061212_052350.cif
_cod_data_source_block           ma3045
_cod_depositor_comments
;
 Changing the capitalization of '_atom_type_symbol' data item
 values and the values of related data items (e. g. _atom_site_type_symbol).
 Updating the _chemical_formula_sum data item value.

 Antanas Vaitkus,
 2017-01-04

The following automatic conversions were performed:
'_refine_ls_structure_factor_coef' value 'fsqd' changed to 'Fsqd'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

'_atom_site_adp_type' value 'uani' changed to 'Uani'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 
(18 times).

'_atom_site_adp_type' value 'uiso' changed to 'Uiso' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (28 times).

'_atom_site_refinement_flags' value 'r' changed to 'R' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (20 times).

'_atom_site_refinement_flags' value 'p' changed to 'P' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (4 times).

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

The following automatic conversions were performed:

'_atom_site_refinement_flags' value 'pr' changed to 'PR' according to
the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (6 times).

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_original_formula_sum        'c16 h23 n o'
_cod_database_code               4022603