Structural, Computational, and Spectroscopic Investigation of [Pd(κ3-1,1′-bis(di-tert-butylphosphino)ferrocenediyl)X]+ (X = Cl, Br, I) Compounds
Blass, Brittany L.; Hernández Sánchez, Raúl; Decker, Victoria A.; Robinson, Michael J.; Piro, Nicholas A.; Kassel, W. Scott; Diaconescu, Paula L.; Nataro, Chip; Organometallics 35 (2016) 462–; doi:10.1021/acs.organomet.5b00889

data_4088161
_publ_section_title
;
 Structural, Computational, and Spectroscopic Investigation of
 [Pd(\k3-1,1&#x2032;-bis(di-tert-butylphosphino)ferrocenediyl)X]+ (X = Cl,
 Br, I) Compounds
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              462
_journal_paper_doi               10.1021/acs.organomet.5b00889
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C51 H46 B Br Cl2 F20 Fe P2 Pd'
_chemical_formula_weight         1424.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.320(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2700(9)
_cell_length_b                   20.0595(11)
_cell_length_c                   18.9011(13)
_cell_measurement_reflns_used    7978
_cell_measurement_temperature    176(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.16
_cell_volume                     5409.0(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      176(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_number            45213
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.358
_diffrn_reflns_theta_min         1.480
_exptl_absorpt_coefficient_mu    1.603
_exptl_absorpt_correction_T_max  0.745210
_exptl_absorpt_correction_T_min  0.593266
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         9863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0534P)^2^+1.1832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7352
_reflns_number_total             9863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00889_si_002.cif
_cod_data_source_block           twin4_175K
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088161
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.740
_shelx_estimated_absorpt_t_max   0.856
_shelx_res_checksum              61685
_shelx_hkl_checksum              58104