Six-fold oxygen-coordinated triplet (S = 1) palladium(II) moieties templated by tris(bipyridine)ruthenium(II) ions.
Pointillart, Fabrice; Train, Cyrille; Villain, Françoise; Moulin, Christophe Cartier Dit; Gredin, Patrick; Chamoreau, Lise-Marie; Gruselle, Michel; Aullon, Gabriel; Alvarez, Santiago; Verdaguer, Michel; Journal of the American Chemical Society 129 (2007) 1327–1334; doi:10.1021/ja066817v

data_4122032
_publ_section_title
;
 Six-fold oxygen-coordinated triplet (S = 1) palladium(II) moieties
 templated by tris(bipyridine)ruthenium(II) ions.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1327
_journal_page_last               1334
_journal_paper_doi               10.1021/ja066817v
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         '2(C30 H24 N6 Ru), 2(Cl6 Pd2), H2 O'
_chemical_formula_sum            'C30 H25 Cl6 N6 O0.5 Pd2 Ru'
_chemical_formula_weight         1004.13
_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                101.751(11)
_cell_angle_beta                 111.493(9)
_cell_angle_gamma                113.567(11)
_cell_formula_units_Z            4
_cell_length_a                   16.302(3)
_cell_length_b                   16.465(3)
_cell_length_c                   16.551(2)
_cell_measurement_reflns_used    148
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      21.8
_cell_measurement_theta_min      3.5
_cell_volume                     3454.8(12)
_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    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0780
_diffrn_reflns_av_sigmaI/netI    0.1220
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            82373
_diffrn_reflns_theta_full        32.00
_diffrn_reflns_theta_max         32.00
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.959
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.758
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         23610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0317P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                12248
_reflns_number_total             23610
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066817vsi20060921_103107.cif
_cod_data_source_block           ct127
_cod_original_cell_volume        3454.8(11)
_cod_database_code               4122032
_cod_duplicate_entry 4109052