Palladium(0) complexes of diferrocenylmercury diphosphines: synthesis, X-ray structure analyses, catalytic isomerization, and C-Cl bond activation.
Tagne Kuate, Alain C.; Lalancette, Roger A.; Bockfeld, Dirk; Tamm, Matthias; Jäkle, Frieder; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4512–4518; doi:10.1039/d1dt00641j

data_7706714
_publ_section_title
;
 Palladium(0) complexes of diferrocenylmercury diphosphines: synthesis,
 X-ray structure analyses, catalytic isomerization, and C-Cl bond
 activation.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4512
_journal_page_last               4518
_journal_paper_doi               10.1039/d1dt00641j
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C61 H50 Fe2 Hg O P2 Pd'
_chemical_formula_sum            'C61 H50 Fe2 Hg O P2 Pd'
_chemical_formula_weight         1279.64
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-01-04 deposited with the CCDC.	2021-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.9860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.56920(10)
_cell_length_b                   12.8337(2)
_cell_length_c                   20.1024(3)
_cell_measurement_reflns_used    33085
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.1520
_cell_measurement_theta_min      2.2010
_cell_volume                     2467.26(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_publication_material
'OLEX2 v1.2 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'
_computing_structure_refinement
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_structure_solution
'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44271
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.844
_diffrn_reflns_theta_min         2.199
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.909
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_description       needle
_exptl_crystal_F_000             1264
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/decane'
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.014
_refine_diff_density_max         1.150
_refine_diff_density_min         -2.501
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details
;
 Flack x determined using 4606 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         10288
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0716P)^2^+2.2559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                10041
_reflns_number_total             10288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00641j2.cif
_cod_data_source_block           at03db
_cod_depositor_comments
'Adding full bibliography for 7706713--7706715.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7706714
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.198
_shelx_estimated_absorpt_t_max   0.829
_oxdiff_exptl_absorpt_empirical_full_min 0.714
_oxdiff_exptl_absorpt_empirical_full_max 1.773
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_shelx_res_checksum              47844
_shelx_hkl_checksum              39759