Synthesis of hydrazinoheterocycles from Morita-Baylis-Hillman adducts of nitroalkenes with azodicarboxylates.
Mane, Vaijinath; Pandey, Jyoti; Ayyagari, Narasihmam; Dey, Chandan; Kale, Raju; Namboothiri, Irishi N. N.; Organic & biomolecular chemistry 14 (2016) 2427–2438; doi:10.1039/c5ob02656c

data_7154919
_publ_section_title
;
 Synthesis of hydrazinoheterocycles from Morita-Baylis-Hillman adducts of
 nitroalkenes with azodicarboxylates.
;
_journal_issue                   8
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2427
_journal_page_last               2438
_journal_paper_doi               10.1039/c5ob02656c
_journal_volume                  14
_journal_year                    2016
_chemical_formula_moiety         'C16 H27 N3 O6'
_chemical_formula_sum            'C16 H27 N3 O6'
_chemical_formula_weight         357.41
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2015-12-24 deposited with the CCDC.
2016-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                102.265(7)
_cell_angle_beta                 100.480(6)
_cell_angle_gamma                90.508(8)
_cell_formula_units_Z            2
_cell_length_a                   9.777(5)
_cell_length_b                   10.159(5)
_cell_length_c                   10.306(5)
_cell_measurement_reflns_used    3091
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.30
_cell_measurement_theta_min      3.00
_cell_volume                     982.4(8)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b28'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b28'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
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_diffrn_reflns_theta_full        29.30
_diffrn_reflns_theta_max         29.30
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_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             384.00
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_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.130
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_refine_diff_density_min         -0.240
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         5353
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_refine_ls_shift/su_max          0.075
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1670
_reflns_number_gt                2442
_reflns_number_total             5353
_reflns_threshold_expression     F>2.0\s(F)
_cod_data_source_file            c5ob02656c3.cif
_cod_data_source_block           INN-MVD-CYCLOHEXYL
_cod_depositor_comments
'Adding full bibliography for 7154918--7154919.cif.'
_cod_original_cell_volume        982.4(9)
_cod_database_code               7154919