A direct access to heterobimetallic complexes by roll-over cyclometallation
Schön, Florian; Leist, Marko; Neuba, Adam; Lang, Johannes; Braun, Carolin; Sun, Yu; Niedner-Schatterburg, Gereon; Braese, Stefan; Thiel, Werner R.; Chem. Commun.  (2017) –; doi:10.1039/C7CC07119A

data_7120767
_publ_section_title
;
 A direct access to heterobimetallic complexes by roll-over
 cyclometallation
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC07119A
_journal_year                    2017
_chemical_formula_sum            'C22 H27 Cl9 Ir N5 Pt'
_chemical_formula_weight         1067.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2014/7
_audit_update_record
;
2017-09-11 deposited with the CCDC.
2017-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                66.417(7)
_cell_angle_beta                 79.935(6)
_cell_angle_gamma                85.543(6)
_cell_formula_units_Z            2
_cell_length_a                   8.7625(7)
_cell_length_b                   13.8954(10)
_cell_length_c                   14.7185(10)
_cell_measurement_reflns_used    4139
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.6980
_cell_measurement_theta_min      5.5810
_cell_volume                     1617.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Giacovazzo et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1399
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1361
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5463
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        62.807
_diffrn_reflns_theta_max         62.807
_diffrn_reflns_theta_min         3.318
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    22.858
_exptl_absorpt_correction_T_max  0.244
_exptl_absorpt_correction_T_min  0.018
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.193
_exptl_crystal_description       prism
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.457
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.130
_refine_diff_density_max         4.306
_refine_diff_density_min         -3.600
_refine_diff_density_rms         0.576
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.379
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.379
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.1095
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2854
_refine_ls_wR_factor_ref         0.2927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4834
_reflns_number_total             5463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07119a2.cif
_cod_data_source_block           shelx_CCDC1
_cod_database_code               7120767
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.034
_shelx_estimated_absorpt_t_max   0.155
_shelx_res_checksum              87979