Synthesis of Mono-, Di-, and Tripalladated 1,3,5-Benzenetricarboxaldehyde Complexes
Vicente, José; Shenoy, Rashmi V.; Martínez-Viviente, Eloísa; Jones, Peter G.; Organometallics 28 (2009) 6101–; doi:10.1021/om9005966

data_4070062
_publ_section_title
;
 Synthesis of Mono-, Di-, and Tripalladated 1,3,5-Benzenetricarboxaldehyde
 Complexes
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              6101
_journal_paper_doi               10.1021/om9005966
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C24 H51 Cu I N9 P3, 3(H2 O), 3(I)'
_chemical_formula_sum            'C24 H57 Cu I4 N9 O3 P3'
_chemical_formula_weight         1183.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   21.059(1)
_cell_length_b                   21.059
_cell_length_c                   15.2873(7)
_cell_measurement_reflns_used    7021
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.3934
_cell_measurement_theta_min      2.8895
_cell_volume                     5871.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34154
_diffrn_reflns_theta_full        32.44
_diffrn_reflns_theta_max         32.44
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    3.875
_exptl_absorpt_correction_T_max  0.7369
_exptl_absorpt_correction_T_min  0.5894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3444
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.519
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         4563
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0449P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                4286
_reflns_number_total             4563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9005966_si_002.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRIGONAL' changed to 'trigonal'
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 
;
_cod_original_cell_volume        5871.2(3)
_cod_original_sg_symbol_H-M      'R 3 c:H'
_cod_database_code               4070062