Reactivity of Bis(pyridyl)-N-alkylaminato Methylpalladium Complexes toward Ethylene: Insights from Experiment and Theory
Swarts, Andrew J.; Zheng, Feng; Smith, Vincent J.; Nordlander, Ebbe; Mapolie, Selwyn F.; Organometallics 33 (2014) 2247–; doi:10.1021/om5001293

data_4083071
_publ_section_title
;
 Reactivity of Bis(pyridyl)-N-alkylaminato Methylpalladium Complexes
 toward Ethylene: Insights from Experiment and Theory
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2247
_journal_paper_doi               10.1021/om5001293
_journal_volume                  33
_journal_year                    2014
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C51 H35 B F24 N4 Pd'
_chemical_formula_sum            'C51 H35 B F24 N4 Pd'
_chemical_formula_weight         1277.04
_chemical_name_common            3e
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.847(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7402(18)
_cell_length_b                   16.231(2)
_cell_length_c                   22.091(3)
_cell_measurement_reflns_used    8469
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.66
_cell_measurement_theta_min      2.19
_cell_volume                     5222.4(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'X-Seed (Atwood & Barbour, 2003)'
_computing_publication_material  'X-Seed (Atwood & Barbour, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_pressure         101.3
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32618
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         1.56
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART Apex'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.8813
_exptl_absorpt_correction_T_min  0.8507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'symmetry-related measurements'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2544
_exptl_crystal_recrystallization_method Dichloromethane
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         12137
_refine_ls_number_restraints     1053
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+13.9389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1783
_reflns_number_gt                9392
_reflns_number_total             12137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5001293_si_001.cif
_cod_data_source_block           C:\3e.CIF
_cod_depositor_comments
;Adding full bibliography for 4083070--4083072.cif.

The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        5222.3(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4083071