Synthesis and characterisation of Pd(ii) and Au(i) complexes with mesoionic carbene ligands bearing phosphinoferrocene substituents and isomeric carbene moieites.
Škoch, Karel; Vosáhlo, Petr; Císařová, Ivana; Štěpnička, Petr; Dalton transactions (Cambridge, England : 2003) 49 (2020) 1011–1021; doi:10.1039/c9dt04521j

data_7703191
_publ_section_title
;
 Synthesis and characterisation of Pd(ii) and Au(i) complexes with
 mesoionic carbene ligands bearing phosphinoferrocene substituents and
 isomeric carbene moieites.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1011
_journal_page_last               1021
_journal_paper_doi               10.1039/c9dt04521j
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         ' C64 H58 Cl2 Fe2 N6 P2 Pd, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C66 H61 B2 Cl2 F8 Fe2 N7 P2 Pd'
_chemical_formula_weight         1476.77
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-11-22 deposited with the CCDC.	2020-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.734(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6351(4)
_cell_length_b                   20.9593(7)
_cell_length_c                   14.0487(5)
_cell_measurement_reflns_used    9720
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.33
_cell_volume                     3124.87(19)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service vV6.2.4'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'PLATON (Spek, 2016)'
_computing_publication_material  'PLATON (Spek, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_radiation_source         'I\mS micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29410
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.025
_diffrn_reflns_theta_min         2.151
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       plate
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 5091 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     828
_refine_ls_number_reflns         12178
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0523
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                11369
_reflns_number_total             12178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04521j2.cif
_cod_data_source_block           mo_ks676
_cod_depositor_comments
'Adding full bibliography for 7703178--7703193.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7703191
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.840
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              92811