A Trialkylphosphine-Derived Palladacycle as a Catalyst in the Selective Cross-Dimerization of Terminal Arylacetylenes with Terminal Propargyl Alcohols and Amides
Lauer, Matthew G.; Headford, Benjamin R.; Gobble, Olivia M.; Weyhaupt, Michelle B.; Gerlach, Deidra L.; Zeller, Matthias; Shaughnessy, Kevin H.; ACS Catalysis 6 (2016) 5834–; doi:10.1021/acscatal.6b01541

data_4513930
_publ_section_title
;
 A Trialkylphosphine-Derived Palladacycle as a Catalyst in the Selective
 Cross-Dimerization of Terminal Arylacetylenes with Terminal Propargyl
 Alcohols and Amides
;
_journal_issue                   9
_journal_name_full               'ACS Catalysis'
_journal_page_first              5834
_journal_paper_doi               10.1021/acscatal.6b01541
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C39 H70 O2 P2 Pd2'
_chemical_formula_sum            'C39 H70 O2 P2 Pd2'
_chemical_formula_weight         845.69
_chemical_name_common            MGL-8-090
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.385(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.7885(3)
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_cell_length_c                   26.2822(9)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.7929
_cell_measurement_theta_min      2.2672
_cell_volume                     8436.5(5)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       11
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_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            137700
_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_full        25.242
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_diffrn_reflns_theta_min         1.463
_diffrn_source                   'sealed X-ray tube'
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_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/5 (Bruker AXS Inc., 2014)'
_exptl_crystal_colour            yellow
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_exptl_crystal_description       rod
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_exptl_crystal_size_min          0.160
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_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         18057
_refine_ls_number_restraints     381
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+6.7621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16180
_reflns_number_total             18057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b01541_si_002.cif
_cod_data_source_block           MGL1_0m_MZ2
_cod_depositor_comments          'Adding full bibliography for 4513930.cif.'
_cod_database_code               4513930
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.631
_shelx_estimated_absorpt_t_max   0.862
_shelx_res_checksum              65711
_shelx_hkl_checksum              9235