Comparison of the catalytic activity for the Suzuki‒Miyaura reaction of (η5-Cp)Pd(IPr)Cl with (η3-cinnamyl)Pd(IPr)(Cl) and (η3-1-t-Bu-indenyl)Pd(IPr)(Cl)
Melvin, Patrick R.; Hazari, Nilay; Lant, Hannah M. C.; Peczak, Ian L.; Shah, Hemali P.; Beilstein Journal of Organic Chemistry 11 (2015) 2476–; doi:10.3762/bjoc.11.269

data_4031800
_publ_section_title
;
 Comparison of the catalytic activity for the Suzuki--Miyaura reaction of
 (\h5-Cp)Pd(IPr)Cl with (\h3-cinnamyl)Pd(IPr)(Cl) and
 (\h3-1-t-Bu-indenyl)Pd(IPr)(Cl)
;
_journal_name_full               'Beilstein Journal of Organic Chemistry'
_journal_page_first              2476
_journal_paper_doi               10.3762/bjoc.11.269
_journal_volume                  11
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C59 H77 Cl N4 Pd2'
_chemical_formula_sum            'C59 H77 Cl N4 Pd2'
_chemical_formula_weight         1090.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.473(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5881(2)
_cell_length_b                   12.3150(2)
_cell_length_c                   19.3155(14)
_cell_measurement_reflns_used    38877
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      63.8
_cell_measurement_theta_min      2.3
_cell_volume                     2710.5(2)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_molecular_graphics
; 
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
OLEX2: A complete structure solution, refinement and analysis program 
(2009). J. Appl. Cryst., 42, 339-341. 
;
_computing_publication_material  'SHELXL-2013/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            90929
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        63.677
_diffrn_reflns_theta_max         63.677
_diffrn_reflns_theta_min         2.326
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    6.101
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.454(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         8645
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0218
_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^)+(0.0294P)^2^+0.5085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0556
_reflns_Friedel_coverage         0.900
_reflns_friedel_fraction_full    0.996
_reflns_friedel_fraction_max     0.996
_reflns_number_gt                8627
_reflns_number_total             8645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1860-5397-11-269-S2.cif
_cod_data_source_block           CpDim
_cod_database_code               4031800
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.581
_shelx_estimated_absorpt_t_max   0.750
_shelx_res_checksum              35363
_shelx_hkl_checksum              49119