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_4065614
_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_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C37 H43 N2, B1 F4 '
_chemical_formula_sum            'C37 H43 B F4 N2'
_chemical_formula_weight         602.57
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 97.2605(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7832(2)
_cell_length_b                   17.7852(4)
_cell_length_c                   21.1308(5)
_cell_measurement_reflns_used    30896
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     3274.40(13)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.070
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30869
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         5.15
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             1280.
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0513
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         3378
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.006398
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979)
0.738    0.558    0.409    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0603
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                3378
_reflns_number_total             7441
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            om1000327_si_003.cif
_cod_data_source_block           Salt_3b
_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_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C37 H43 B1 F4 N2 '
_cod_database_code               4065614