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_7113397
_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            'C29 H29 Ir N3 P'
_chemical_formula_weight         642.72
_chemical_name_common            'compound 5'
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_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                92.45(5)
_cell_angle_beta                 102.39(4)
_cell_angle_gamma                98.18(2)
_cell_formula_units_Z            2
_cell_length_a                   9.341(5)
_cell_length_b                   9.958(5)
_cell_length_c                   13.571(9)
_cell_measurement_reflns_used    4059
_cell_measurement_temperature    213
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     1216.9(12)
_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 0.646
_diffrn_measured_fraction_theta_max 0.646
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4773
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    5.575
_exptl_absorpt_correction_T_max  0.572
_exptl_absorpt_correction_T_min  0.344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.213
_refine_diff_density_min         -2.076
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0584
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1468
_reflns_number_gt                2686
_reflns_number_total             3595
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b409514f.txt
_cod_data_source_block           compound_5
_cod_original_cell_volume        1216.9(13)
_cod_original_sg_symbol_H-M      'P -1         '
_cod_database_code               7113397