Synthesis and Structure of Dinuclear Silver(I) and Palladium(II) Complexes of 2,7-Bis(methylene)naphthalene-Bridged Bis-N-Heterocyclic Carbene Ligands
Saito, Shinichi; Saika, Mitsuya; Yamasaki, Ryu; Azumaya, Isao; Masu, Hyuma; Organometallics 30 (2011) 1366–; doi:10.1021/om1008583

data_4063697
_publ_section_title
;
 Synthesis and Structure of Dinuclear Silver(I) and Palladium(II)
 Complexes of 2,7-Bis(methylene)naphthalene-Bridged Bis-N-Heterocyclic
 Carbene Ligands
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1366
_journal_paper_doi               10.1021/om1008583
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C52 H64 N8 I4 Pd2, 2(C H2 Cl2)'
_chemical_formula_sum            'C54 H68 Cl4 I4 N8 Pd2'
_chemical_formula_weight         1691.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 130.5370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.0351(8)
_cell_length_b                   9.8429(2)
_cell_length_c                   23.6265(6)
_cell_measurement_reflns_used    8052
_cell_measurement_temperature    150
_cell_measurement_theta_max      65.35
_cell_measurement_theta_min      2.54
_cell_volume                     6192.0(3)
_computing_cell_refinement       'Smart (Bruker AXS)'
_computing_data_collection       'Smart '
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Bruker ApexII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25841
_diffrn_reflns_theta_full        66.03
_diffrn_reflns_theta_max         66.03
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    22.251
_exptl_absorpt_correction_T_max  0.1351
_exptl_absorpt_correction_T_min  0.0949
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.254
_refine_diff_density_min         -1.372
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0754P)^2^+68.0042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                4571
_reflns_number_total             4980
_reflns_threshold_expression     >2sigma
_cod_data_source_file            om1008583_si_002.cif
_cod_data_source_block           a0504221mas(9b)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        6192.0(2)
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               4063697