Diferrocenylmercury diphosphine diastereomers with unique geometries: trans-chelation at Pd(ii) with short Hg(ii)Pd(ii) contacts.
Tagne Kuate, Alain C.; Lalancette, Roger A.; Bannenberg, Thomas; Tamm, Matthias; Jäkle, Frieder; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13430–13439; doi:10.1039/c9dt02728a

data_7700844
_publ_section_title
;
 Diferrocenylmercury diphosphine diastereomers with unique geometries:
 trans-chelation at Pd(ii) with short Hg(ii)Pd(ii) contacts.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13430
_journal_page_last               13439
_journal_paper_doi               10.1039/c9dt02728a
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_formula_moiety         '2(C44 H36 Cl2 Fe2 Hg P2 Pd), C7 H8'
_chemical_formula_sum            'C95 H80 Cl4 Fe4 Hg2 P4 Pd2'
_chemical_formula_weight         2324.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-08-13 deposited with the CCDC.    2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_length_b                   10.733(2)
_cell_length_c                   17.663(4)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.18
_cell_measurement_theta_min      2.54
_cell_volume                     4047.4(15)
_computing_cell_refinement       'APEX 2'
_computing_data_collection       'APEX 2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker SMART CCD Apex-II area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19025
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.781
_diffrn_reflns_theta_min         2.539
_exptl_absorpt_coefficient_mu    18.040
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_exptl_absorpt_correction_T_min  0.168
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_description       block
_exptl_crystal_F_000             2268
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, hexanes'
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Flack x determined using 2517 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         6757
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0282
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0446
_refine_ls_wR_factor_ref         0.0458
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    0.851
_reflns_Friedel_fraction_max     0.834
_reflns_number_gt                6321
_reflns_number_total             6757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02728a2.cif
_cod_data_source_block           5b
_cod_depositor_comments
'Adding full bibliography for 7700841--7700844.cif.'
_cod_original_cell_volume        4047.6(14)
_cod_database_code               7700844
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.187
_shelx_estimated_absorpt_t_max   0.266
_shelx_res_checksum              68772