An unexpected three-component reaction of 2-alkylenecyclobutanone, N'-(2-alkynylbenzylidene)hydrazide with water
Pan, Xiaolin; Wang, He; xia, hongguang; Wu, Jie; RSC Adv.  (2015) –; doi:10.1039/C5RA17787A

data_7222353
_publ_section_title
;
 An unexpected three-component reaction of 2-alkylenecyclobutanone,
 N'-(2-alkynylbenzylidene)hydrazide with water
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA17787A
_journal_year                    2015
_chemical_formula_sum            'C27 H22 N2 O2'
_chemical_formula_weight         406.46
_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   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-06-29 deposited with the CCDC.
2015-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                72.789(4)
_cell_angle_beta                 81.884(4)
_cell_angle_gamma                68.844(4)
_cell_formula_units_Z            2
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_cell_length_b                   10.741(3)
_cell_length_c                   11.550(3)
_cell_measurement_reflns_used    3722
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.31
_cell_volume                     1044.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7562
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         1.847
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
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_exptl_crystal_description       prism
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_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.340
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_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4712
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.1141P)^2^+0.2645P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3752
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           mo_41215a
_cod_original_cell_volume        1044.5(4)
_cod_database_code               7222353
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_shelxl_version_number           2013-2
_shelx_res_checksum              70481