Synthesis of Spiropentadiene Pyrazolones by Rh(III)-Catalyzed Formal sp(3) C-H Activation/Annulation.
Zheng, Jiuan; Li, Panpan; Gu, Meng; Lin, Aijun; Yao, Hequan; Organic letters 19 (2017) 2829–2832; doi:10.1021/acs.orglett.7b00930

data_1546231
_publ_section_title
;
 Synthesis of Spiropentadiene Pyrazolones by Rh(III)-Catalyzed Formal
 sp(3) C-H Activation/Annulation.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2829
_journal_page_last               2832
_journal_paper_doi               10.1021/acs.orglett.7b00930
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C34 H28 N2 O2'
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_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
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_symmetry_space_group_name_Hall  '-P 1'
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_cell_angle_beta                 86.158(2)
_cell_angle_gamma                85.402(2)
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_cell_length_a                   9.9922(18)
_cell_length_b                   19.110(4)
_cell_length_c                   21.951(4)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.65
_cell_measurement_theta_min      2.16
_cell_volume                     4168.6(14)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
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_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
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_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         0.930
_exptl_absorpt_coefficient_mu    0.074
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1033
_refine_ls_number_reflns         14656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1500P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
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_reflns_number_total             14656
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b00930_si_003.cif
_cod_data_source_block           as
_cod_original_cell_volume        4168.7(13)
_cod_database_code               1546231
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2013-2
_shelx_res_checksum              46642
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