Palladium(II) Pyrazolin-4-ylidenes: Substituent Effects on the Formation and Catalytic Activity of Pyrazole-Based Remote NHC Complexes
Han, Yuan; Lee, Li Juan; Huynh, Han Vinh; Organometallics 28 (2009) 2778–; doi:10.1021/om8010849

data_4068778
_publ_section_title
;
 Palladium(II) Pyrazolin-4-ylidenes: Substituent Effects on the Formation
 and Catalytic Activity of Pyrazole-Based Remote NHC Complexes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2778
_journal_paper_doi               10.1021/om8010849
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C21 H28 I2 N3 O0.5 Pd'
_chemical_formula_weight         690.66
_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                 99.156(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.577(2)
_cell_length_b                   9.4289(11)
_cell_length_c                   28.349(3)
_cell_measurement_reflns_used    8393
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.28
_cell_volume                     4902.4(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26478
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    3.289
_exptl_absorpt_correction_T_max  0.5592
_exptl_absorpt_correction_T_min  0.2603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.193
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         11178
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0344P)^2^+11.9167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                8811
_reflns_number_total             11178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8010849_si_002.cif
_cod_data_source_block           5c
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not Measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4902.5(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C21 H28 I2 N3 O0.50 Pd'
_cod_database_code               4068778