Selective synthesis of isomeric heterodinuclear complexes with switched metal arrangements via proton-induced reversible metal migration.
Dubs, Christian; Inagaki, Akiko; Akita, Munetaka; Chemical communications (Cambridge, England)  (2004) 2760–2761; doi:10.1039/b409514f

data_7113396
_publ_section_title
;
 Selective synthesis of isomeric heterodinuclear complexes with switched
 metal arrangements via proton-induced reversible metal migration.
;
_journal_issue                   23
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2760
_journal_page_last               2761
_journal_paper_doi               10.1039/b409514f
_journal_year                    2004
_chemical_formula_sum            'C32.5 H35 B Cl F4 Ir N3 P Pd'
_chemical_formula_weight         919.47
_chemical_name_common            'compound 4a BF4'
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_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                83.74(4)
_cell_angle_beta                 79.66(3)
_cell_angle_gamma                88.57(3)
_cell_formula_units_Z            4
_cell_length_a                   13.877(9)
_cell_length_b                   14.786(13)
_cell_length_c                   16.189(14)
_cell_measurement_reflns_used    12471
_cell_measurement_temperature    213
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3248(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.803
_diffrn_measured_fraction_theta_max 0.803
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1828
_diffrn_reflns_av_sigmaI/netI    0.3832
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18654
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    4.829
_exptl_absorpt_correction_T_max  0.616
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.809
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.662
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         11925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.662
_refine_ls_R_factor_all          0.2412
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.2056
_reflns_number_gt                3480
_reflns_number_total             11925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b409514f.txt
_cod_data_source_block           compound_4a
_cod_original_formula_sum        'C32.50 H35 B Cl F4 Ir N3 P Pd'
_cod_database_code               7113396