Hemilabile and Bimetallic Coordination in Rh and Ir Complexes of NCN Pincer Ligands.
Mancano, Giulia; Page, Michael J.; Bhadbhade, Mohan; Messerle, Barbara A.; Inorganic chemistry 53 (2014) 10159–10170; doi:10.1021/ic501158x

data_4341142
_publ_section_title
;
 Hemilabile and Bimetallic Coordination in Rh and Ir Complexes of NCN
 Pincer Ligands.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10159
_journal_page_last               10170
_journal_paper_doi               10.1021/ic501158x
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
'(C30 H36 Ir N12), (C24 H20 B), 0.5(C H2 Cl2)'
_chemical_formula_sum            'C54.5 H57 B Cl Ir N12'
_chemical_formula_weight         1118.58
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                92.8470(10)
_cell_angle_beta                 102.154(2)
_cell_angle_gamma                94.3120(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3367(3)
_cell_length_b                   12.8201(4)
_cell_length_c                   19.6142(7)
_cell_measurement_reflns_used    9819
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.499
_cell_measurement_theta_min      2.603
_cell_volume                     2528.05(14)
_computing_cell_refinement       '<i>APEX2 </i>(Bruker, 2007)'
_computing_data_collection       '<i>APEX2 </i>(Bruker, 2007)'
_computing_data_reduction        '<i>APEX2 </i>(Bruker, 2007)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.0266
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35831
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.023
_exptl_absorpt_coefficient_mu    2.744
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            'Orange red'
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       Cubes
_exptl_crystal_F_000             1134
_exptl_crystal_size_max          0.361
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.210
_refine_diff_density_max         2.217
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         8907
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+5.3383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8566
_reflns_number_total             8907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501158x_si_001.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 4341139--4341144.cif.'
_cod_original_formula_sum        'C54.50 H57 B Cl Ir N12'
_cod_database_code               4341142
_shelx_estimated_absorpt_t_min   0.437
_shelx_estimated_absorpt_t_max   0.597
_shelxl_version_number           2013-4
_shelx_res_checksum              38114
_shelx_hkl_checksum              40843