Triphenylphosphine-mediated reaction of dialkyl azodicarboxylate with activated alkenes leading to pyrazolines
Yamazaki, Shoko; Maenaka, Yuta; Fujinami, Ken; Mikata, Yuji; RSC Advances 2 (2012) 8095–; doi:10.1039/c2ra21249h

data_7238703
_publ_section_title
;
 Triphenylphosphine-mediated reaction of dialkyl azodicarboxylate with
 activated alkenes leading to pyrazolines
;
_journal_issue                   21
_journal_name_full               'RSC Advances'
_journal_page_first              8095
_journal_paper_doi               10.1039/c2ra21249h
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety         'C19 H30 N2 O9'
_chemical_formula_sum            'C19 H30 N2 O9'
_chemical_formula_weight         430.45
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                99.6509(16)
_cell_angle_beta                 96.6679(14)
_cell_angle_gamma                112.7480(15)
_cell_formula_units_Z            2
_cell_length_a                   9.2138(15)
_cell_length_b                   9.2556(15)
_cell_length_c                   14.723(3)
_cell_measurement_reflns_used    3262
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.05
_cell_volume                     1118.7(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_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      123
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0122
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8677
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       unknown
_exptl_crystal_F_000             460.00
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.580
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4855
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0885P)^2^+0.6683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1697
_reflns_number_gt                4302
_reflns_number_total             4855
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2ra21249h.txt
_cod_data_source_block           524X-1-110527-2
_cod_original_cell_volume        1118.7(4)
_cod_database_code               7238703