Mono- and Dinuclear Five-coordinate Cyclometalated Palladium(II) Compounds
Margarita López-Torres; Alberto Fernández; Jesús J. Fernández; Antonio Suárez; M Teresa Pereira; Juan M. Ortigueira; José M. Vila; H. Adams; Inorganic Chemistry 40 (2001) 4583–4587; doi:10.1021/ic001094g

data_4320139
_publ_contact_author_address
;
      Departamento de Quimica Inorganica
      Universidad de Santiago de Compostela
      E-15076 Santiago de Compostela
      SPAIN
;
_publ_contact_author_name        'Dr. Jose M. Vila'
_publ_section_title
;
 Mono- and Dinuclear Five-coordinate Cyclometalated Palladium(II)
 Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4583
_journal_page_last               4587
_journal_paper_doi               10.1021/ic001094g
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C47 H44.5 Cl2.5 N2 O4.5 P3 Pd'
_chemical_formula_weight         997.28
_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
_cell_angle_alpha                98.710(10)
_cell_angle_beta                 97.73(3)
_cell_angle_gamma                100.22(2)
_cell_formula_units_Z            4
_cell_length_a                   13.527(6)
_cell_length_b                   17.542(5)
_cell_length_c                   20.100(6)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.819
_cell_measurement_theta_min      9.919
_cell_volume                     4575(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18308
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        16.32
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.703
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.033
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1073
_refine_ls_number_reflns         16062
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.030
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.1139
_refine_ls_R_factor_obs          0.0677
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+5.8239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1987
_refine_ls_wR_factor_obs         0.1652
_reflns_number_observed          10273
_reflns_number_total             16069
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001094g_2.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+5.8239P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+5.8239P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4575.4(28)
_cod_original_formula_sum        'C47 H44.50 Cl2.50 N2 O4.50 P3 Pd'
_cod_database_code               4320139