Palladium complexes of ferrocene-based phosphine ligands as redox-switchable catalysts in Buchwald‒Hartwig cross-coupling reactions
Feyrer, Alexander; Breher, Frank; Inorganic Chemistry Frontiers 4 (2017) 1125–; doi:10.1039/C7QI00125H

data_4349688
_publ_section_title
;
 Palladium complexes of ferrocene-based phosphine ligands as
 redox-switchable catalysts in Buchwald--Hartwig cross-coupling reactions
;
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1125
_journal_paper_doi               10.1039/C7QI00125H
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C35 H32 Fe N O3 P Pd S, C4 H8 O'
_chemical_formula_sum            'C39 H40 Fe N O4 P Pd S'
_chemical_formula_weight         812.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-03 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.814(5)
_cell_length_b                   10.271(2)
_cell_length_c                   14.863(3)
_cell_measurement_reflns_used    31983
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.000
_cell_measurement_theta_min      1.785
_cell_volume                     3482.7(12)
_computing_cell_refinement       'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_data_collection       'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)'
_computing_data_reduction        'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector, \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0900
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31983
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.785
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_T_max  0.443
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 2573 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7549
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0394P)^2^+5.0270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                6397
_reflns_number_total             7549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qi00125h2.cif
_cod_data_source_block           sad_a
_cod_database_code               4349688
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.672
_shelx_estimated_absorpt_t_max   0.774
_shelx_res_checksum              35570
_shelx_hkl_checksum              26062