Palladium and Platinum Acyl Complexes and Their Lewis Acid Adducts. Experimental and Computational Study of Thermodynamics and Bonding
Chen, Danmin; Gau, Michael R.; Dobereiner, Graham E.; Organometallics 34 (2015) 4069–; doi:10.1021/acs.organomet.5b00507

data_4086190
_publ_section_title
;
 Palladium and Platinum Acyl Complexes and Their Lewis Acid Adducts.
 Experimental and Computational Study of Thermodynamics and Bonding
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4069
_journal_paper_doi               10.1021/acs.organomet.5b00507
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C75 H49 B F24 P2 Pd'
_chemical_formula_sum            'C75 H49 B F24 P2 Pd'
_chemical_formula_weight         1585.29
_chemical_melting_point          ?
_chemical_name_common
'Bistriphenylphosphine Benzyl Palladium(II) BArF'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                71.819(2)
_cell_angle_beta                 84.345(2)
_cell_angle_gamma                86.986(2)
_cell_formula_units_Z            2
_cell_length_a                   12.9724(11)
_cell_length_b                   15.0893(14)
_cell_length_c                   18.0910(17)
_cell_measurement_reflns_used    9500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.575
_cell_measurement_theta_min      2.304
_cell_volume                     3347.2(5)
_computing_cell_refinement       'SAINT (Bruker-AXS)'
_computing_data_collection       'COSMO (Bruker-AXS)'
_computing_data_reduction        'SADABS (Bruker-AXS)'
_computing_molecular_graphics    XP
_computing_publication_material  'APEX2 Report Generator (Bruker-AXS)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'fine-focused sealed tube'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47480
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.976
_diffrn_reflns_theta_min         1.189
_diffrn_source                   'Kappa APEX II DUO'
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
47480 Corrected reflections written to file mo_2053_0m.hkl
 Estimated minimum and maximum transmission:  0.6674  0.7456
 The ratio of these values is more reliable than their absolute values!
 Additional spherical absorption correction applied with mu*r =  0.2000
 Lambda/2 correction factor = 0.0015
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          .169
_exptl_crystal_size_mid          .163
_exptl_crystal_size_min          .070
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.098
_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     928
_refine_ls_number_reflns         16025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0645P)^2^+1.7835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11899
_reflns_number_total             16025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00507_si_002.cif
_cod_data_source_block           solvefinal
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not determined' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4086190.cif.
;
_cod_original_cell_volume        3347.1(5)
_cod_database_code               4086190
_shelxl_version_number           2013-3
_shelx_res_checksum              5691
_shelx_hkl_checksum              31749