Highly peri-, regio- and diastereoselective 1,3-dipolar cycloaddition of mesitonitrile oxide to 1,7-dimethyl-2,3-dihydro-1H-1,4-diazepines: unexpected one-step formation of a new triheterocyclic framework
Baouid, Abdesselam; Elhazazi, Saïd; Hasnaoui, Aïssa; Compain, Philippe; Lavergne, Jean-Pierre; Huet, François; New Journal of Chemistry 25 (2001) 1479–1481; doi:10.1039/B107409C

data_7052473
_publ_section_title
;
 Highly peri-, regio- and diastereoselective 1,3-dipolar cycloaddition
 of mesitonitrile oxide to 1,7-dimethyl-2,3-dihydro-1H-1,4-diazepines:
 unexpected one-step formation of a new triheterocyclic framework
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1479
_journal_page_last               1481
_journal_paper_doi               10.1039/B107409C
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C33 H38 N4 O2'
_chemical_formula_weight         522.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_type_scat_source           'Waasmaier & Kirfel (1995)'
_cell_angle_alpha                90.000(10)
_cell_angle_beta                 101.078(3)
_cell_angle_gamma                90.000(10)
_cell_formula_units_Z            4
_cell_length_a                   22.9235(7)
_cell_length_b                   9.9309(5)
_cell_length_c                   12.8363(7)
_cell_measurement_reflns_used    11268
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      1
_cell_volume                     2867.7(2)
_computing_data_collection       'KappaCCD Reference Manual (Nonius, 1998)'
_computing_data_reduction        'maXus (Mackay et al., 1998)'
_computing_molecular_graphics    maXus
_computing_publication_material  maXus
_computing_structure_refinement  maXus
_computing_structure_solution    maXus
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       \f
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .071
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4771
_diffrn_reflns_theta_max         24.19
_exptl_absorpt_coefficient_mu    .077
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.20
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'thin plate'
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .10
_refine_diff_density_max         .21
_refine_diff_density_min         -.33
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.575
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     352
_refine_ls_number_reflns         3640
_refine_ls_R_factor_gt           .073
_refine_ls_shift/esd_mean        .00065
_refine_ls_shift/su_max          .0037
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F~o~^2^) + 0.03F~o~^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .083
_reflns_number_gt                3640
_reflns_number_total             4280
_reflns_threshold_expression     refl_observed_if_I_>_1.75\s(I)
_cod_data_source_file            b107409c.txt
_cod_data_source_block           I
_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:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 39 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 'w = 1/[\s^2^(F~o~^2^) +
0.03F~o~^2^]' 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^(F~o~^2^) + 0.03F~o~^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2867.8(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7052473