Cyclometalated Palladium(II) Fragments as Building Blocks in the Construction of New Heteronuclear Metalomacrocycles
López-Torres, Margarita; Fernández, Alberto; Fernández, Jesús J.; Suárez, Antonio; Castro-Juiz, Samuel; Vila, José M.; Pereira, M. Teresa; Organometallics 20 (2001) 1350–; doi:10.1021/om000840m

data_4077234
_publ_section_title
;
 Cyclometalated Palladium(II) Fragments as Building Blocks in the
 Construction of New Heteronuclear Metalomacrocycles
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1350
_journal_paper_doi               10.1021/om000840m
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C112 H115 Br4 Cl9 Fe2 N4 P4 Pd4'
_chemical_formula_weight         2816.95
_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                 90.4070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.32380(10)
_cell_length_b                   27.1937(3)
_cell_length_c                   17.93870(10)
_cell_measurement_reflns_used    154
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      1.10
_cell_volume                     12353.13(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42391
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.10
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.383
_exptl_absorpt_correction_T_max  0.4490
_exptl_absorpt_correction_T_min  0.3820
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            orangge
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5616
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.327
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         15240
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0958P)^2^+60.4589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.1862
_reflns_number_gt                10307
_reflns_number_total             15240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000840m.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4077234