Synthesis, crystal structure, solution and spectroscopic properties, and hydrogen-evolving activity of [K(18-crown-6)][Pt(ii)(2-phenylpyridinato)Cl2]
Kobayashi, Masayuki; Masaoka, Shigeyuki; Sakai, Ken; Photochemical & Photobiological Sciences 8 (2009) 196–; doi:10.1039/b814939a

data_1515951
_publ_section_title
;
 Synthesis, crystal structure, solution and spectroscopic properties, and
 hydrogen-evolving activity of
 [K(18-crown-6)][Pt(ii)(2-phenylpyridinato)Cl2]
;
_journal_issue                   2
_journal_name_full
'Photochemical &amp; Photobiological Sciences'
_journal_page_first              196
_journal_paper_doi               10.1039/b814939a
_journal_volume                  8
_journal_year                    2009
_chemical_formula_moiety
'C23 H34 Cl2 K N O7 Pt, C23 H32 Cl2 K N O6 Pt'
_chemical_formula_sum            'C46 H66 Cl4 K2 N2 O13 Pt2'
_chemical_formula_weight         1465.19
_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
_cell_angle_alpha                110.600(2)
_cell_angle_beta                 103.178(2)
_cell_angle_gamma                92.221(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6085(18)
_cell_length_b                   14.149(2)
_cell_length_c                   19.981(4)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.21
_cell_volume                     2710.1(8)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'KENX (Sakai, 2002)'
_computing_publication_material
;
SHELXL97, TEXSAN (Molecular Structure Corporation, 2001),
KENX, and ORTEP (Johnson, 1976)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device
'Bruker SMART APEX CCD-detector diffractometer'
_diffrn_measurement_method       \w
_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  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26240
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    5.568
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, G. M., 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         6.780
_refine_diff_density_min         -4.533
_refine_ls_extinction_expression not_refined
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         9847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0533P)^2^+61.7929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1580
_refine_ls_wR_factor_ref         0.1632
_reflns_number_gt                8188
_reflns_number_total             9847
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b814939a.txt
_cod_data_source_block           071221ptppycl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_database_code               1515951