Gold/Gallium-Catalyzed Annulation of 1,3-Dicarbonyl Com-pounds and Cyclopropylacetylenes for Synthesis of Substi-tuted Cyclopentenes
Shi, Xiaodong; Dong, Boliang; Xi, Yumeng; Su, Yijin; Ahkmedov, Novruz G.; Petersen, Jeffrey L.; RSC Adv.  (2016) –; doi:10.1039/C6RA00896H

data_7224148
_publ_section_title
;
 Gold/Gallium-Catalyzed Annulation of 1,3-Dicarbonyl Com-pounds and
 Cyclopropylacetylenes for Synthesis of Substi-tuted Cyclopentenes
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA00896H
_journal_year                    2016
_chemical_formula_sum            'C17 H20 N4 O6'
_chemical_formula_weight         376.37
_chemical_name_systematic
'(E)-ethyl 1-(1-(2-(2,4-dinitrophenyl)hydrazono)ethyl)-2-methylcyclopent-2-enecarboxylate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2015-11-03 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                84.514(2)
_cell_angle_beta                 89.785(2)
_cell_angle_gamma                81.048(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3303(6)
_cell_length_b                   7.9078(6)
_cell_length_c                   16.0868(13)
_cell_measurement_reflns_used    8418
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6277
_cell_measurement_theta_min      3.0206
_cell_volume                     916.86(13)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Buker AXS D8 Venture fixed-chi'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14534
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.80
_diffrn_source_type              fine-focus
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/3 (Bruker AXS Inc.)'
_exptl_crystal_colour            'intense yellow'
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             396
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_size_max          0.579
_exptl_crystal_size_mid          0.433
_exptl_crystal_size_min          0.274
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+1.0768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1883
_reflns_number_gt                2367
_reflns_number_total             3425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra00896h2.cif
_cod_data_source_block           I
_cod_database_code               7224148
_shelx_res_checksum              1262