Pd(II)-Catalyzed alkyne annulation through allylic isomerization: synthesis of spiro-cyclopentadiene pyrazolones.
Changmai, Sumi; Sultana, Sabera; Sarma, Bipul; Gogoi, Sanjib; Chemical communications (Cambridge, England) 57 (2021) 6027–6030; doi:10.1039/d1cc02155a

data_7128382
_publ_section_title
;
 Pd(II)-Catalyzed alkyne annulation through allylic isomerization:
 synthesis of spiro-cyclopentadiene pyrazolones.
;
_journal_issue                   49
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6027
_journal_page_last               6030
_journal_paper_doi               10.1039/d1cc02155a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_sum            'C39 H30 N2 O'
_chemical_formula_weight         542.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-08-01 deposited with the CCDC.	2021-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                76.694(3)
_cell_angle_beta                 86.042(3)
_cell_angle_gamma                85.353(3)
_cell_formula_units_Z            4
_cell_length_a                   10.9996(6)
_cell_length_b                   12.1270(6)
_cell_length_c                   23.4345(12)
_cell_measurement_reflns_used    6617
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.75
_cell_measurement_theta_min      2.19
_cell_volume                     3028.0(3)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_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  0.1002
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            101889
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.819
_diffrn_reflns_theta_min         1.729
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         15450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.0606
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7364
_reflns_number_total             15450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02155a2.cif
_cod_data_source_block           SC25
_cod_depositor_comments
'Adding full bibliography for 7128382--7128383.cif.'
_cod_database_code               7128382
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              1435
_shelx_hkl_checksum              80172