Pd-Catalyzed Spirocyclization via C-H Activation and Benzyne Insertion.
Yoon, Hyung; Lossouarn, Alexis; Landau, Felicitas; Lautens, Mark; Organic letters 18 (2016) 6324–6327; doi:10.1021/acs.orglett.6b03213

data_1555958
_publ_section_title
;
 Pd-Catalyzed Spirocyclization via C-H Activation and Benzyne Insertion.
;
_journal_issue                   24
_journal_name_full               'Organic letters'
_journal_page_first              6324
_journal_page_last               6327
_journal_paper_doi               10.1021/acs.orglett.6b03213
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C52 H43 N O P2 Pd, C H Cl3'
_chemical_formula_sum            'C53 H44 Cl3 N O P2 Pd'
_chemical_formula_weight         985.58
_space_group_crystal_system      monoclinic
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_cell_angle_beta                 103.385(3)
_cell_angle_gamma                90
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_cell_length_a                   11.7599(10)
_cell_length_b                   18.0933(13)
_cell_length_c                   23.3373(19)
_cell_measurement_reflns_used    9754
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.25
_cell_volume                     4830.7(7)
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_computing_data_collection       'APEX2 (Bruker, 2014)'
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_diffrn_ambient_temperature      147(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
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_diffrn_reflns_theta_full        25.242
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_diffrn_reflns_theta_min         1.439
_diffrn_source
'sealed tube with Bruker Triumph monochromator'
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       Block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.180
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_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         11135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+4.7756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0660
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_reflns_number_gt                9046
_reflns_number_total             11135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b03213_si_001.cif
_cod_data_source_block           d16110_a_sq
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1555958
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.869
_shelx_estimated_absorpt_t_max   0.891
_shelx_res_checksum              36625
_shelx_hkl_checksum              53320
_shelx_fab_checksum              17530