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_4065613
_publ_section_title
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 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         ' C31 H31 N2, C1 H2 Cl2, B1 F4 '
_chemical_formula_sum            'C32 H33 B Cl2 F4 N2'
_chemical_formula_weight         603.34
_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
_cell_angle_alpha                90
_cell_angle_beta                 93.1091(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2656(2)
_cell_length_b                   9.7269(2)
_cell_length_c                   25.0605(3)
_cell_measurement_reflns_used    30789
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     2985.47(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  0.037
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            30789
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         5.10
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             1256.
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.87
_refine_diff_density_min         -1.05
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0438
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         3941
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.004115
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979)
 1.43    0.910    0.852    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0827
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                3941
_reflns_number_total             6775
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            om1000327_si_002.cif
_cod_data_source_block           Salt_3a
_cod_depositor_comments
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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 

The following automatic conversions were performed:
data name '_geom_contact__publ_flag' replaced with
'_geom_contact_publ_flag' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 5005 2017-03-03 11:38:54Z antanas 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C32 H33 B1 Cl2 F4 N2 '
_cod_database_code               4065613