Metal-Mediated Transformation of a Triazinephenanthridinium Ligand Leading to a {Pd5} Coordination Complex Observed Crystallographically and by Cryospray Mass Spectrometry
Phil J. Kitson; Yu-Fei Song; Patrick Gamez; Paul de Hoog; De-Liang Long; Alexis D. C. Parenty; Jan Reedijk; Leroy Cronin; Inorganic Chemistry 47 (2008) 1883–1885; doi:10.1021/ic7022192

data_4304669
_publ_section_title
;
Metal-Mediated Transformation of a Triazinephenanthridinium Ligand Leading
to a {Pd5} Coordination Complex Observed Crystallographically and by
Cryospray Mass Spectrometry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1883
_journal_page_last               1885
_journal_paper_doi               10.1021/ic7022192
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety
'(C96 H92 N24 O18 Pd5 2+), 2(Br -), 5(H2 O), 6(C H2 Cl2)'
_chemical_formula_sum            'C102 H114 Br2 Cl12 N24 O23 Pd5'
_chemical_formula_weight         3161.39
_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-97
_cell_angle_alpha                84.276(2)
_cell_angle_beta                 86.994(2)
_cell_angle_gamma                83.200(2)
_cell_formula_units_Z            1
_cell_length_a                   11.9704(6)
_cell_length_b                   15.7849(6)
_cell_length_c                   21.4407(10)
_cell_measurement_reflns_used    7570
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      48.13
_cell_measurement_theta_min      4.54
_cell_volume                     3999.3(3)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       '\w & \p 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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0770
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34772
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.310
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1582
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.23
_refine_diff_density_min         -1.01
_refine_diff_density_rms         0.20
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         14352
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0869
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1568P)^2^+24.4691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2489
_refine_ls_wR_factor_ref         0.2879
_reflns_number_gt                9234
_reflns_number_total             14352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7022192-file001.cif
_cod_data_source_block           pk341a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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_database_code               4304669