Functionalized 2-Pyridyl-Substituted Metallo-1,2-enedithiolates. Synthesis, Characterization, and Photophysical Properties of (dppe)M{S2C2(2-pyridine(ium))(CH2CH2OR'')} and (dppe)M[{S2C2(CH2CH2-N-2-pyridinium)}]+ (R'' = H, Acetyl, Lauroyl; M = Pd, Pt; dppe = 1,2-Bis(diphenylphosphino)ethane)
Kelly A. Van Houten; Danica C. Heath; Chris A. Barringer; Arnold L. Rheingold; Robert S. Pilato; Inorganic Chemistry 37 (1998) 4647–4653; doi:10.1021/ic980273j

data_4323000
_publ_contact_author
;
     Dr. Robert S. Pilato
     Chemistry Department
     University of Maryland, College Park
     College Park, Maryland 20742 400076
     USA
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_publ_contact_author_email       rp78@umail.umd.edu
_publ_contact_author_fax         301-314-9121
_publ_contact_author_phone       301-405-7022
_publ_section_title
;
 Functionalized 2-Pyridyl-Substituted Metallo-1,2-enedithiolates.
 Synthesis, Characterization, and Photophysical Properties of
 (dppe)M{S2C2(2-pyridine(ium))(CH2CH2OR'')} and
 (dppe)M[{S2C2(CH2CH2-N-2-pyridinium)}]+ (R'' = H, Acetyl, Lauroyl; M =
 Pd, Pt; dppe = 1,2-Bis(diphenylphosphino)ethane)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4647
_journal_page_last               4653
_journal_paper_doi               10.1021/ic980273j
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C59 H52 B N P2 Pd S2'
_chemical_formula_weight         1018.29
_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                106.292(2)
_cell_angle_beta                 96.235(2)
_cell_angle_gamma                95.183(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1924(2)
_cell_length_b                   16.0181(2)
_cell_length_c                   17.4368(3)
_cell_measurement_reflns_used    5546
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      3.0
_cell_volume                     2430.09(8)
_computing_cell_refinement       SAINT
_computing_data_collection       'Siemens P4/CCD'
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      218(2)
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       'phi, omega'
_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  0.0686
_diffrn_reflns_av_sigmaI/netI    0.1418
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11821
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.23
_diffrn_standards_decay_%        <1.0
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       blade
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.0011(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.139
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         7210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_restrained_S_obs      1.139
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_obs          0.0642
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1560
_refine_ls_wR_factor_obs         0.1180
_reflns_number_observed          4478
_reflns_number_total             7214
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980273j.cif
_cod_data_source_block           pilo
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] 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^)+(0.0300P)^2^+0.0000P] 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        2430.09(7)
_cod_database_code               4323000