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_4068936
_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            'C52 H68 Cl2 N4 O7 Pd'
_chemical_formula_weight         1038.40
_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                76.52(2)
_cell_angle_beta                 72.01(2)
_cell_angle_gamma                81.22(3)
_cell_formula_units_Z            2
_cell_length_a                   11.831(3)
_cell_length_b                   13.697(4)
_cell_length_c                   18.135(4)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      7.24
_cell_measurement_theta_min      4.54
_cell_volume                     2707.7(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       Omega/2-Theta
_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  0.0100
_diffrn_reflns_av_sigmaI/netI    0.0797
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10281
_diffrn_reflns_theta_full        25.26
_diffrn_reflns_theta_max         25.26
_diffrn_reflns_theta_min         1.20
_diffrn_standards_decay_%        0.633
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.9376
_exptl_absorpt_correction_T_min  0.9282
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         1.331
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     mixed
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         9757
_refine_ls_number_restraints     6
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_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0676P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1594
_reflns_number_gt                5379
_reflns_number_total             9757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8011695_si_004.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^)+(0.0676P)^2^+0.0000P] 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^)+(0.0676P)^2^+0.0000P] 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        2707.9(12)
_cod_database_code               4068936