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_4088159
_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_moiety         'C26 H44 Br Fe P2 Pd, C H2 Cl2, B C24 F20'
_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_date             2016-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.728(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.177(3)
_cell_length_b                   20.023(3)
_cell_length_c                   18.731(4)
_cell_measurement_reflns_used    5213
_cell_measurement_temperature    78(2)
_cell_measurement_theta_max      25.669
_cell_measurement_theta_min      2.401
_cell_volume                     5314.7(18)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      78.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_number            7586
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        23.450
_diffrn_reflns_theta_max         23.450
_diffrn_reflns_theta_min         1.489
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.631
_exptl_absorpt_correction_T_max  0.744893
_exptl_absorpt_correction_T_min  0.499468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0841 before and 0.0616 after correction.
 The Ratio of minimum to maximum transmission is 0.67.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1162 before and 0.0731 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 40499 reflections, Rint = 0.0876
 (12395 with I > 3sig(I), Rint = 0.0572)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.231
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         7586
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0647P)^2^+0.4746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5605
_reflns_number_total             7586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00889_si_002.cif
_cod_data_source_block           twin4_80k
_cod_original_cell_volume        5314.9(16)
_cod_database_code               4088159
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.736
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C62, C83
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C62 \\sim C83: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C62) \\sim Ueq, Uanis(C83) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Fe1) = Uanis(Fe1B)
Uanis(Pd1) = Uanis(Pd1B)
Uanis(Br1) = Uanis(Br1B)
4. Others
 Sof(Pd1B)=Sof(Br1B)=Sof(Fe1B)=1-FVAR(1)
 Sof(Pd1)=Sof(Br1)=Sof(Fe1)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
5.b Me refined with riding coordinates:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10)
;
_shelx_res_checksum              40260
_shelx_hkl_checksum              53303
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'