Synthesis of Pt(dpk)Cl4 and the Reversible Hydration to Pt(dpk-O-OH)Cl3.H-phenCl: X-ray, Spectroscopic, and Electrochemical Characterization
Katherine N. Crowder; Stephanie J. Garcia; Rebekah L. Burr; J. Micah North; Mike H. Wilson; Brian L. Conley; Phillip E. Fanwick; Peter S. White; Karl D. Sienerth; Robert M. Granger; Inorganic Chemistry 43 (2004) 72–78; doi:10.1021/ic035102f

data_4310363
_publ_contact_author
;
     P.E. Fanwick
     Department of Chemistry
     Purdue University
     W. Lafayette
     IN 47907
     USA
;
_publ_contact_author_email       fanwick@.xray.chem.purdue.edu
_publ_contact_author_fax         '(317) 494 0239'
_publ_contact_author_phone       '(317) 494 4572'
_publ_section_title
;
 Synthesis of Pt(dpk)Cl4 and the Reversible Hydration to
 Pt(dpk-O-OH)Cl3.H-phenCl: X-ray, Spectroscopic, and Electrochemical
 Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              72
_journal_page_last               78
_journal_paper_doi               10.1021/ic035102f
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C23 H18 Cl4 N4 O2 Pt'
_chemical_formula_weight         719.33
_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_type_scat_source           International_Tables_for_Xray_Crystallography
_audit_creation_date             14-03-96
_audit_creation_method           from_MolEN_master_file_using_cif_in
_cell_angle_alpha                100.346(12)
_cell_angle_beta                 95.190(10)
_cell_angle_gamma                115.117(13)
_cell_formula_units_Z            2
_cell_length_a                   8.2320(11)
_cell_length_b                   8.7139(14)
_cell_length_c                   19.097(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      21
_cell_measurement_theta_min      19
_cell_volume                     1198.6(3)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        PROCESS_MolEN_(Fair,_1990)
_computing_molecular_graphics    ORTEP_(Johnson,_1976)
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  LSFM_MolEN_(Fair,_1990)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      295
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       Enraf_Nonius_CAD4
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6061
_diffrn_reflns_theta_max         27.82
_diffrn_reflns_theta_min         2.68
_diffrn_standards_interval_time  83
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.393
_exptl_absorpt_correction_T_max  0.3752
_exptl_absorpt_correction_T_min  0.2458
_exptl_absorpt_correction_type   refined_empirical_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.99
_exptl_crystal_description       plate
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.91
_refine_diff_density_min         -0.26
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.190
_refine_ls_hydrogen_treatment
;
Chemically significant hydrogens refined isotropically
Others not refined, U=1.3*Ueq of bonding atom
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4767
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_obs          0.031
_refine_ls_shift/esd_max         0.011
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.038
_reflns_number_observed          4767
_reflns_number_total             5669
_reflns_observed_criterion       >3.0\s(I)
_cod_data_source_file            ic035102fsi20030917_050934.cif
_cod_data_source_block           DPKPHE
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/ (\s^2^(Fo^2^) + 0.0016
Fo^4^)' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w = 4Fo^2^/
(\s^2^(Fo^2^) + 0.0016 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1198.6(7)
_cod_original_formula_sum        'C23 H18 Cl4 N4 O2 Pt1'
_cod_database_code               4310363