Palladium(II)−N-Heterocyclic Carbene Metallacrown Ether Complexes: Synthesis, Structure, and Catalytic Activity in the Suzuki−Miyaura Reaction
Zhang, Xiaoqin; Qiu, Yuping; Rao, Bin; Luo, Meiming; Organometallics 28 (2009) 3093–; doi:10.1021/om8011695

data_4068935
_publ_section_title
;
 Palladium(II)&#x2212;N-Heterocyclic Carbene Metallacrown Ether Complexes:
 Synthesis, Structure, and Catalytic Activity in the Suzuki&#x2212;Miyaura
 Reaction
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              3093
_journal_paper_doi               10.1021/om8011695
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C47 H56 Cl4 N4 O6 Pd'
_chemical_formula_weight         1021.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.76(4)
_cell_angle_beta                 81.41(3)
_cell_angle_gamma                89.16(3)
_cell_formula_units_Z            2
_cell_length_a                   12.849(3)
_cell_length_b                   14.526(4)
_cell_length_c                   14.563(4)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      7.74
_cell_measurement_theta_min      4.54
_cell_volume                     2406.6(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       Omega/2-Thteta
_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  0.0075
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9145
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        1.365
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.8901
_exptl_absorpt_correction_T_min  0.8751
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         8934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+0.8501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                6139
_reflns_number_total             8934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8011695_si_003.cif
_cod_data_source_block           cd4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+0.8501P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+0.8501P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2406.6(11)
_cod_database_code               4068935