Unprecedented eight-palladium(i) crown-cycle with metal?metal unsupported bonds
Angurell, Inma; Mart�nez-Ruiz, Isabel; Rossell, Oriol; Seco, Miquel; G�mez-Sal, Pilar; Mart�n, Avelino; Chemical Communications  (2004) 1712–1713; doi:10.1039/b405532b

data_7111323
_publ_section_title
;
 Unprecedented eight-palladium(i) crown-cycle with metal?metal unsupported
 bonds
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1712
_journal_page_last               1713
_journal_paper_doi               10.1039/b405532b
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C52 H57 Cl9 N12 P4 Pd4'
_chemical_formula_sum            'C52.5 H56.5 Cl10 N12 P4 Pd4'
_chemical_formula_weight         1759.58
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-03-01T11:45:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.257(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.541(11)
_cell_length_b                   17.474(4)
_cell_length_c                   24.144(2)
_cell_measurement_reflns_used    377
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.938
_cell_measurement_theta_min      3.074
_cell_measurement_wavelength     0.71073
_cell_volume                     13465(6)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1075
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            71813
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.588
_exptl_absorpt_correction_T_max  0.5039
_exptl_absorpt_correction_T_min  0.4491
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6956
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.511
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         13853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.083
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+213.8975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1408
_reflns_number_gt                10142
_reflns_number_total             13853
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b405532bsup1.cif
_cod_data_source_block           miquel2
_cod_original_formula_sum        'C52.50 H56.50 Cl10 N12 P4 Pd4'
_cod_database_code               7111323
_exptl_absorpt_correction_t_ave  0.4422