Palladium-mediated intramolecular dearomatization of ligated dialkylterphenyl phosphines.
Rama, Raquel J.; Maya, Celia; Nicasio, M. Carmen; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14575–14579; doi:10.1039/c9dt03201k

data_7700941
_publ_section_title
;
 Palladium-mediated intramolecular dearomatization of ligated
 dialkylterphenyl phosphines.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14575
_journal_page_last               14579
_journal_paper_doi               10.1039/c9dt03201k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C34 H40 Cl P Pd'
_chemical_formula_sum            'C34 H40 Cl P Pd'
_chemical_formula_weight         621.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-08-02 deposited with the CCDC.    2019-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.1371(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8449(6)
_cell_length_b                   13.4470(6)
_cell_length_c                   15.8973(6)
_cell_measurement_reflns_used    8003
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.95
_cell_measurement_theta_min      2.29
_cell_volume                     2986.9(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26078
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         22.041
_diffrn_reflns_theta_min         1.656
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.5960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0730 before and 0.0371 after correction. The Ratio of minimum to maximum transmission is 0.8003. The \l/2 correction factor is 0.0000.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1320
_exptl_crystal_recrystallization_method
'Crystallised from a mixture of dichloromethane, pentane and hexane by cooling'
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         7465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+5.4964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6011
_reflns_number_total             7465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03201k2.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 7700939--7700941.cif.'
_cod_database_code               7700941
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.955
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              37075
_shelx_fab_checksum              34915