Synthesis, Structure, and Temperature-Dependent Dynamics of Neutral Palladium Allyl Complexes of Annulated Diaminocarbenes and Their Catalytic Application for C−C and C−N Bond Formation Reactions†
Dastgir, Sarim; Coleman, Karl S.; Cowley, Andrew R.; Green, Malcolm L. H.; Organometallics 29 (2010) 4858–; doi:10.1021/om1000327

data_4065615
_publ_section_title
;
 Synthesis, Structure, and Temperature-Dependent Dynamics of Neutral
 Palladium Allyl Complexes of Annulated Diaminocarbenes and Their
 Catalytic Application for C&#x2212;C and C&#x2212;N Bond Formation
 Reactions&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4858
_journal_paper_doi               10.1021/om1000327
_journal_volume                  29
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C40 H47 Cl1 N2 Pd1 '
_chemical_formula_sum            'C40 H47 Cl N2 Pd'
_chemical_formula_weight         697.68
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7787(2)
_cell_length_b                   14.8681(2)
_cell_length_c                   21.6983(3)
_cell_measurement_reflns_used    34581
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     3477.34(9)
_computing_cell_refinement
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
KappaCCD software 'Collect' (Nonius, 2000) 
;
_computing_data_reduction
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_publication_material
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_refinement
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; 
Nonius KappaCCD 
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            34581
_diffrn_reflns_theta_full        27.480
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         5.247
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' pale yellow '
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       ' fragment '
_exptl_crystal_F_000             1446.000
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.90
_refine_diff_density_min         -1.05
_refine_ls_abs_structure_details 'Flack, 3452 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.06(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1049
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6456
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.043927
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.209 0.174E-01 -0.504E-02 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0494
_refine_ls_wR_factor_gt          0.0327
_refine_ls_wR_factor_ref         0.0327
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                6456
_reflns_number_total             7835
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            om1000327_si_004.cif
_cod_data_source_block           Palladium_Complex_5b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        ' C40 H47 Cl1 N2 Pd1 '
_cod_database_code               4065615