Monodentate phosphine substitution in [Pd(κ(3)-dppf)(PR3)][BF4]2 (dppf = 1,1'-bis(diphenylphosphino)ferrocene) compounds.
Cabrera, K. D.; Rowland, A. T.; Szarko, J. M.; Diaconescu, P. L.; Bezpalko, M. W.; Kassel, W. S.; Nataro, C.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5702–5710; doi:10.1039/c6dt04921d

data_7042215
_publ_section_title
;
 Monodentate phosphine substitution in [Pd(\k(3)-dppf)(PR3)][BF4]2 (dppf =
 1,1'-bis(diphenylphosphino)ferrocene) compounds.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5702
_journal_page_last               5710
_journal_paper_doi               10.1039/c6dt04921d
_journal_volume                  46
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C52.00 H40.00 B2 F11 Fe1 P3 Pd1'
_chemical_formula_sum            'C52 H40 B2 F11 Fe P3 Pd'
_chemical_formula_weight         1150.66
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-09
_audit_creation_method           CRYSTALS_ver_14.61_build_00000
_audit_update_record
;
2017-02-10 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9819(15)
_cell_length_b                   16.6637(14)
_cell_length_c                   17.6944(15)
_cell_measurement_reflns_used    9789
_cell_measurement_temperature    100
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     5302.0(8)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14303
_diffrn_reflns_theta_full        29.160
_diffrn_reflns_theta_max         29.160
_diffrn_reflns_theta_min         1.666
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2312.001
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/diethyl ether'
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.180
_platon_squeeze_details
;
TITL chip118_0ma in Pna2(1)
CELL   17.9820   16.6640   17.6940     90.00     90.00     90.00
SPGR Pna21
C101 0.188 0.424 0.522 !       6.08 eA-3
C102 0.760 0.171 0.399 !       5.68 eA-3
C103 0.755 0.106 0.495 !       4.79 eA-3
C104 0.309 0.960 0.089 !       4.23 eA-3
C105 0.619 0.079 0.402 !       3.71 eA-3
Q106 0.112 0.481 0.628 !       3.53 eA-3
C107 0.783 0.562 0.915 !       2.30 eA-3
Q108 0.045 0.429 0.431 !       1.99 eA-3
C109 0.309 0.898 0.923 !       1.97 eA-3
Q110 0.909 0.846 0.000 !       1.66 eA-3
C111 0.191 0.895 0.069 !       1.59 eA-3
Q112 0.234 0.829 0.099 !       1.31 eA-3
Q113 0.109 0.437 0.591 !       1.12 eA-3
Q114 0.114 0.192 0.951 !       1.06 eA-3
Q115 0.093 0.686 0.949 !       1.04 eA-3
Q116 0.109 0.492 0.371 !       0.99 eA-3
Q117 0.628 0.504 0.073 !       0.95 eA-3
Q118 0.833 0.980 0.971 !       0.89 eA-3
Q119 0.832 0.986 0.031 !       0.89 eA-3
Q120 0.149 0.430 0.640 !       0.89 eA-3
Q121 0.951 0.359 0.500 !       0.88 eA-3
Q122 0.405 0.188 0.561 !       0.87 eA-3
Q123 0.861 0.268 0.459 !       0.84 eA-3
Q124 0.128 0.704 0.007 !       0.82 eA-3
Q125 0.749 0.106-0.002 !       0.80 eA-3
Q126 0.859 0.263 0.551 !       0.73 eA-3
Q127 0.126 0.704 0.086 !       0.73 eA-3
Q128 0.976 0.625 0.263 !       0.72 eA-3
Q129 0.614 0.309 0.051 !       0.71 eA-3
Q130 0.260 0.389 0.630 !       0.70 eA-3
Q131 0.467 0.988 0.087 !       0.68 eA-3
Q132 0.659 0.550 0.065 !       0.68 eA-3
C133 0.098 0.452 0.514 !       0.62 eA-3
Q134 0.130 0.077 0.935 !       0.62 eA-3
C135 0.892 0.457 0.100 !       0.62 eA-3
Q136 0.263 0.987 0.884 !       0.61 eA-3
Q137 0.362 0.637 0.411 !       0.61 eA-3
Q138 0.829 0.968 0.877 !       0.60 eA-3
Q139 0.327 0.533 0.123 !       0.59 eA-3
Q140 0.946 0.930 0.517 !       0.58 eA-3
Q141 0.548 0.403 0.038 !       0.58 eA-3
Q142 0.547 0.403 0.972 !       0.57 eA-3
Q143 0.941 0.379 0.439 !       0.56 eA-3
C144 0.606 0.547 0.113 !       0.55 eA-3
C145 0.835 0.657 0.900 !       0.54 eA-3
Q146 0.199 0.637 0.005 !       0.53 eA-3
Q147 0.198 0.027 0.576 !       0.52 eA-3
Q148 0.158 0.097 0.048 !       0.52 eA-3
Q149 0.645 0.938 0.012 !       0.51 eA-3
C150 0.353 0.881 0.942 !       0.50 eA-3
Q151 0.343 0.893 0.852 !       0.50 eA-3
;
_refine_diff_density_max         0.98
_refine_diff_density_min         -0.71
_refine_ls_abs_structure_details 'Flack (1983), 6919 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         14303
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.0166572
_refine_ls_shift/su_mean         0.0006816
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 6.67P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0950
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0950
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              -24
_reflns_number_gt                12467
_reflns_number_total             14303
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0419
_oxford_refine_ls_scale          0.063573(7)
_oxford_reflns_number_all        14303
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'chip118_0ma in Pna2(1)'
_cod_data_source_file            c6dt04921d1.cif
_cod_data_source_block           chip118
_cod_depositor_comments          'Adding full bibliography for 7042215.cif.'
_cod_original_sg_symbol_Hall     'P 2c -2n '
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C52.00 H40.00 B2 F11 Fe1 P3 Pd1'
_cod_database_code               7042215
_platon_squeeze_void_probe_radius 1.20