Inhibited Catalyst Activation in (N-Heterocyclic carbene)PdCl2(diethylamine) Complexes by Intramolecular Hydrogen Bonding
Chen, Ming-Tsz; Vicic, David A.; Chain, William J.; Turner, Michael L.; Navarro, Oscar; Organometallics 30 (2011) 6770–; doi:10.1021/om200828a

data_4065474
_publ_section_title
;
 Inhibited Catalyst Activation in (N-Heterocyclic
 carbene)PdCl2(diethylamine) Complexes by Intramolecular Hydrogen Bonding
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6770
_journal_paper_doi               10.1021/om200828a
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C31 H47 Cl2 N3 Pd, 0.5(C6 H14)'
_chemical_formula_sum            'C34 H54 Cl2 N3 Pd'
_chemical_formula_weight         682.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 105.083(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.799(4)
_cell_length_b                   15.183(4)
_cell_length_c                   19.257(6)
_cell_measurement_reflns_used    11469
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.78
_cell_measurement_theta_min      2.19
_cell_volume                     3613.2(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Rigaku Mercury70 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47538
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.87
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.8637
_exptl_absorpt_correction_T_min  0.7709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.153
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         12685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+1.3022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                10175
_reflns_number_total             12685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200828a_si_001.cif
_cod_data_source_block           IPrPdCl2DEA
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3613.2(18)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4065474