A mixed-valence chloride-bridged (pincer)Ir^III^‒(diene)Ir^I^ complex
Pelczar, Elizabeth M.; Emge, Thomas J.; Goldman, Alan S.; Acta Crystallographica Section C 63 (2007) m323–m326; doi:10.1107/S0108270107022378

data_2016029
_publ_section_title
;
 A mixed-valence chloride-bridged (pincer)Ir^III^--(diene)Ir^I^ complex
;
_journal_coeditor_code           GA3042
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m323
_journal_page_last               m326
_journal_paper_doi               10.1107/S0108270107022378
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ir2 (C8 H12) (C24 H44 P2) Cl2] , 0.5C6 H14'
_chemical_formula_moiety         'C32 H56 Cl2 Ir2 P2 , 0.5C6 H14'
_chemical_formula_sum            'C35 H63 Cl2 Ir2 P2'
_chemical_formula_weight         1001.09
_chemical_name_common
;
\k^3^-(^tBu^PCPIrH)-(\m~2~Cl)~2~-\h^4^-Ir(COD)
;
_chemical_name_systematic
;
[2,6-bis(di-tert-butylphosphino)phenyl-1\k^3^P,C^1^,P']di-\m-chlorido-
1:2\k^4^Cl:Cl-(2\h^4^-cycloocta-2,5-diene)diiridium(I,III) hexane hemisolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.4160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8424(7)
_cell_length_b                   11.6735(5)
_cell_length_c                   22.0589(10)
_cell_measurement_reflns_used    8331
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.56
_cell_volume                     3770.5(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus (Bruker,2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2003)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            42778
_diffrn_reflns_theta_full        30.61
_diffrn_reflns_theta_max         30.61
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.301
_exptl_absorpt_correction_T_max  0.558
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in SAINT-Plus; Bruker, 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.040
_refine_diff_density_min         -1.027
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         11498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0263
_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^)+(0.03P)^2^+7.5P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0622
_reflns_number_gt                10259
_reflns_number_total             11498
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ga3042.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2016029
_cod_database_fobs_code          2016029