Comparing the reactivity of isomeric phosphinoferrocene nitrile and isocyanide in Pd(ii) complexes: synthesis of simple coordination compounds vs. preparation of P-chelated insertion products and Fischer-type carbenes.
Škoch, Karel; Císařová, Ivana; Uhlík, Filip; Štěpnička, Petr; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16082–16101; doi:10.1039/c8dt03564d

data_7047634
_publ_section_title
;
 Comparing the reactivity of isomeric phosphinoferrocene nitrile and
 isocyanide in Pd(ii) complexes: synthesis of simple coordination
 compounds vs. preparation of P-chelated insertion products and
 Fischer-type carbenes.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16082
_journal_page_last               16101
_journal_paper_doi               10.1039/c8dt03564d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C43 H39 Cl Fe N P2 Pd, B F4'
_chemical_formula_sum            'C43 H39 B Cl F4 Fe N P2 Pd'
_chemical_formula_weight         916.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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
;
2018-07-23 deposited with the CCDC.
2018-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.617(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.6324(12)
_cell_length_b                   19.4838(8)
_cell_length_c                   16.5874(7)
_cell_measurement_reflns_used    6899
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      2.48
_cell_volume                     7646.9(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.4'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'PLATON (Spek, 2016)'
_computing_publication_material  'PLATON (Spek, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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  0.0795
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.006
_diffrn_reflns_theta_min         2.478
_exptl_absorpt_coefficient_mu    1.057
_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    1.592
_exptl_crystal_description       bar
_exptl_crystal_F_000             3712
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         7513
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0220P)^2^+31.5545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5594
_reflns_number_total             7513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03564d6.cif
_cod_data_source_block           mo_ks818
_cod_depositor_comments
'Adding full bibliography for 7047627--7047638.cif.'
_cod_database_code               7047634
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.802
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              89354