Stoichiometry controlled self-assembly of tri- and octa-nuclear palladium‒yttrium complexes
Chikkali, Samir H.; Nieger, Martin; Gudat, Dietrich; New Journal of Chemistry 34 (2010) 1348–; doi:10.1039/c0nj00020e

data_7053441
_publ_section_title
;
 Stoichiometry controlled self-assembly of tri- and octa-nuclear
 palladium--yttrium complexes
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1348
_journal_paper_doi               10.1039/c0nj00020e
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety
'C164 H149 N4 O21 P8 Pd4 Y4, 12(C3 H7 N O), 3(Cl), 5(H2 O)'
_chemical_formula_sum            'C200 H243 Cl3 N16 O38 P8 Pd4 Y4'
_chemical_formula_weight         4614.45
_chemical_name_common
;
(mu4-hydroxo-octakis-(mu-3-3-(diphenyl)methyl-1,2-
catecholato)-tetra-(dimethylformamide)-tetra-yttrium(iii)-tetra-
palladium(ii))trichloride dimethylformamide solvate (penta)hydrate
;
_chemical_name_systematic
;
[mu4-hydroxo-octakis-(mu-3-3-(diphenyl)methyl-1,2-catecholato)-tetra-
(dimethylformamide)-tetra-yttrium(III)-tetra-palladium(II)]trichloride
dimethylformamide solvate (penta)hydrate
;
_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                67.152(1)
_cell_angle_beta                 70.115(1)
_cell_angle_gamma                74.181(1)
_cell_formula_units_Z            1
_cell_length_a                   16.3740(2)
_cell_length_b                   18.8825(2)
_cell_length_c                   20.6120(3)
_cell_measurement_reflns_used    121719
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1
_cell_volume                     5449.58(13)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega'
_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  0.1193
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            121719
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    1.541
_exptl_absorpt_correction_T_max  0.8767
_exptl_absorpt_correction_T_min  0.6461
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2370
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.637
_refine_diff_density_min         -1.524
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         26720
_refine_ls_number_restraints     603
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+24.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1931
_refine_ls_wR_factor_ref         0.2138
_reflns_number_gt                19275
_reflns_number_total             26720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00020e.txt
_cod_data_source_block           5Cl3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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        5449.58(12)
_cod_database_code               7053441