Six-fold Oxygen-Coordinated Triplet (S= 1) Palladium(II) Moieties Templated by Tris(bipyridine)ruthenium(II) Ions
Fabrice Pointillart; Cyrille Train; Françoise Villain; Patrick Gredin; Lise-Marie Chamoreau; Michel Gruselle; Gabriel Aullon; Santiago Alvarez; Michel Verdaguer; Journal of the American Chemical Society 129 (2007) 1327–1334; doi:10.1021/ja066817v

data_4109051
_publ_contact_author
;
Cyrille Train
;
_publ_contact_author_email       train@ccr.jussieu.fr
_publ_contact_author_fax         '00 33 1 44 27 38 41'
_publ_contact_author_phone       '00 33 1 44 27 30 59'
_publ_section_title
;
 Six-fold Oxygen-Coordinated Triplet (S= 1) Palladium(II) Moieties
 Templated by Tris(bipyridine)ruthenium(II) Ions
;
_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_absolute_configuration ad
_chemical_formula_moiety
'2(C30 H24 N6 Ru), Cl4 Pd,2(C2 O4) Pd, 11(H2 O)'
_chemical_formula_sum            'C64 H70 Cl4 N12 O19 Pd2 Ru2'
_chemical_formula_weight         1868.08
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-03-09
_audit_creation_method           CRYSTALS_ver_12.82
_cell_angle_alpha                90
_cell_angle_beta                 113.313(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4366(17)
_cell_length_b                   25.409(3)
_cell_length_c                   12.862(3)
_cell_measurement_reflns_used    258
_cell_measurement_temperature    180
_cell_measurement_theta_max      19.9
_cell_measurement_theta_min      4.5
_cell_volume                     3732.6(12)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT. Nonius (1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.08
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25501
_diffrn_reflns_theta_full        25.109
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         2.088
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'DIFABS (Walker & Stuart, 1983)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       parallelepipped
_exptl_crystal_F_000             1854
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.74
_refine_diff_density_min         -2.83
_refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0770
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         11153
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.006819
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.02 0.496 0.682 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0801
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0645
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              32
_reflns_limit_k_min              -32
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                11153
_reflns_number_total             15034
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.1614(2)
_oxford_structure_analysis_title '11270929 Compound X'
_cod_data_source_file            ja066817vsi20060921_103043.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_cell_volume        3732.5(11)
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               4109051