Characterization and Reactivity Studies of Dinuclear Iridium Hydride Complexes Prepared from Iridium Catalysts with N,P and C,N Ligands under Hydrogenation Conditions
Gruber, Stefan; Neuburger, Markus; Pfaltz, Andreas; Organometallics 32 (2013) 4702–; doi:10.1021/om4007467

data_4081469
_publ_section_title
;
 Characterization and Reactivity Studies of Dinuclear Iridium Hydride
 Complexes Prepared from Iridium Catalysts with N,P and C,N Ligands under
 Hydrogenation Conditions
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4702
_journal_paper_doi               10.1021/om4007467
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C32 H12 B F24, C23 H33 Ir N2 O2 P, 1.27(C H2 Cl2)'
_chemical_formula_sum            'C56.28 H47.55 B Cl2.55 F24 Ir N2 O2 P'
_chemical_formula_weight         1560.19
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                67.9070(10)
_cell_angle_beta                 69.4010(10)
_cell_angle_gamma                84.5930(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8192(3)
_cell_length_b                   16.1838(4)
_cell_length_c                   17.2644(4)
_cell_measurement_reflns_used    9069
_cell_measurement_temperature    123
_cell_measurement_theta_max      30
_cell_measurement_theta_min      4
_cell_volume                     3103.56(13)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            116614
_diffrn_reflns_theta_full        28.569
_diffrn_reflns_theta_max         30.073
_diffrn_reflns_theta_min         1.773
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.401
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1535.100
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.52
_refine_diff_density_min         -1.31
_refine_ls_abs_structure_details 'Flack (1983), 17526 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.028(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0761
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1770
_refine_ls_number_reflns         31146
_refine_ls_number_restraints     370
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.0009627
_refine_ls_shift/su_mean         0.0000298
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.462 0.562 0.418 0.184 0.668E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0342
_refine_ls_wR_factor_gt          0.0269
_refine_ls_wR_factor_ref         0.0266
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              24
_reflns_limit_l_min              -24
_reflns_number_gt                31737
_reflns_number_total             35611
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.40
_oxford_diffrn_Wilson_scale      86.05
_oxford_refine_ls_r_factor_ref   0.0259
_oxford_refine_ls_scale          0.10732(4)
_oxford_reflns_number_all        35516
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om4007467_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_formula_sum        'C56.28 H47.55 B1 Cl2.55 F24 Ir1 N2 O2 P1'
_cod_database_code               4081469
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
EQUIVALENCE PART(1001, OCC) 
CONTINUE    PART(1002, OCC) 
WEIGHT -1   PART(1002, OCC) 
EQUIVALENCE PART(2001, OCC) 
CONTINUE    PART(2002, OCC) 
WEIGHT -1   PART(2002, OCC) 
EQUIVALENCE PART(3001, OCC) 
CONTINUE    PART(3002, OCC) 
WEIGHT -1   PART(3002, OCC) 
EQUIVALENCE PART(4001, OCC) 
CONTINUE    PART(4002, OCC) 
WEIGHT -1   PART(4002, OCC) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) H   (  33,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) H   (  43,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) H   (  93,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) H   ( 253,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) H   ( 303,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) H   ( 443,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) H   ( 463,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) 
RIDE C   (  92,X'S) H   ( 921,X'S) 
RIDE C   (  96,X'S) H   ( 961,X'S) 
RIDE C   (  98,X'S) H   ( 981,X'S) 
RIDE C   ( 100,X'S) H   (1001,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 108,X'S) H   (1081,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) H   (1112,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) H   (1122,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) H   (1132,X'S) 
RIDE C   ( 213,X'S) H   (2131,X'S) H   (2132,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
REM 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
REM   ASSEMBLY1   START (DO NOT REMOVE THIS LINE) 
REM   EXTERNAL BONDS 
DISTANCES  0.0 , 0.01  = MEAN 
CONTINUE C(77) TO C(73) C(177) TO C(73) 
REM   INTERNAL BONDS 
DISTANCES  0.0 , 0.01  = MEAN 
CONTINUE C(77) TO F(19) C(177) TO F(119) 
CONTINUE C(77) TO F(20) C(177) TO F(120) 
CONTINUE C(77) TO F(21) C(177) TO F(121) 
REM   ANGLES RESTRAINTS 
ANGLES  0.0 , 0.10  = MEAN 
CONTINUE F(19) TO C(77) TO C(73) F(119) TO C(177) TO C(73) 
CONTINUE F(20) TO C(77) TO C(73) F(120) TO C(177) TO C(73) 
CONTINUE F(20) TO C(77) TO F(19) F(120) TO C(177) TO F(119) 
CONTINUE F(21) TO C(77) TO C(73) F(121) TO C(177) TO C(73) 
CONTINUE F(21) TO C(77) TO F(19) F(121) TO C(177) TO F(119) 
CONTINUE F(21) TO C(77) TO F(20) F(121) TO C(177) TO F(120) 
REM   VIBRATIONAL RESTRAINTS 
VIBRATIONS 0.0, 0.0100  = 
CONTINUE C(77) TO C(73) C(177) TO C(73) 
CONTINUE C(77) TO F(19) C(177) TO F(119) 
CONTINUE C(77) TO F(20) C(177) TO F(120) 
CONTINUE C(77) TO F(21) C(177) TO F(121) 
VIBRATIONS 0.0, 0.00100  = 
CONTINUE C(77) TO C(177) 
CONTINUE F(19) TO F(119) 
CONTINUE F(20) TO F(120) 
CONTINUE F(21) TO F(121) 
REM   SIMILARITY RESTRAINTS 
U(IJ)'S 0.0, 0.0200  = 
CONTINUE C(77) TO C(73) C(177) TO C(73) 
CONTINUE C(77) TO F(19) C(177) TO F(119) 
CONTINUE C(77) TO F(20) C(177) TO F(120) 
CONTINUE C(77) TO F(21) C(177) TO F(121) 
U(IJ)'S 0.0, 0.00200  = 
CONTINUE C(77) TO C(177) 
CONTINUE F(19) TO F(119) 
CONTINUE F(20) TO F(120) 
CONTINUE F(21) TO F(121) 
REM   ASSEMBLY1   END (DO NOT REMOVE THIS LINE) 
REM   ASSEMBLY2   START (DO NOT REMOVE THIS LINE) 
REM   EXTERNAL BONDS 
DISTANCES  0.0 , 0.01  = MEAN 
CONTINUE C(86) TO C(83) C(186) TO C(83) 
REM   INTERNAL BONDS 
DISTANCES  0.0 , 0.01  = MEAN 
CONTINUE C(86) TO F(28) C(186) TO F(128) 
CONTINUE C(86) TO F(29) C(186) TO F(129) 
CONTINUE C(86) TO F(30) C(186) TO F(130) 
REM   ANGLES RESTRAINTS 
ANGLES  0.0 , 0.10  = MEAN 
CONTINUE F(28) TO C(86) TO C(83) F(128) TO C(186) TO C(83) 
CONTINUE F(29) TO C(86) TO C(83) F(129) TO C(186) TO C(83) 
CONTINUE F(29) TO C(86) TO F(28) F(129) TO C(186) TO F(128) 
CONTINUE F(30) TO C(86) TO C(83) F(130) TO C(186) TO C(83) 
CONTINUE F(30) TO C(86) TO F(28) F(130) TO C(186) TO F(128) 
CONTINUE F(30) TO C(86) TO F(29) F(130) TO C(186) TO F(129) 
REM   VIBRATIONAL RESTRAINTS 
VIBRATIONS 0.0, 0.0100  = 
CONTINUE C(86) TO C(83) C(186) TO C(83) 
CONTINUE C(86) TO F(28) C(186) TO F(128) 
CONTINUE C(86) TO F(29) C(186) TO F(129) 
CONTINUE C(86) TO F(30) C(186) TO F(130) 
VIBRATIONS 0.0, 0.00100  = 
CONTINUE C(86) TO C(186) 
CONTINUE F(28) TO F(128) 
CONTINUE F(29) TO F(129) 
CONTINUE F(30) TO F(130) 
REM   SIMILARITY RESTRAINTS 
U(IJ)'S 0.0, 0.0200  = 
CONTINUE C(86) TO C(83) C(186) TO C(83) 
CONTINUE C(86) TO F(28) C(186) TO F(128) 
CONTINUE C(86) TO F(29) C(186) TO F(129) 
CONTINUE C(86) TO F(30) C(186) TO F(130) 
U(IJ)'S 0.0, 0.00200  = 
CONTINUE C(86) TO C(186) 
CONTINUE F(28) TO F(128) 
CONTINUE F(29) TO F(129) 
CONTINUE F(30) TO F(130) 
REM   ASSEMBLY2   END (DO NOT REMOVE THIS LINE) 
REM   ASSEMBLY3   START (DO NOT REMOVE THIS LINE) 
REM   EXTERNAL BONDS 
DISTANCES  0.0 , 0.01  = MEAN 
CONTINUE C(109) TO C(105) C(209) TO C(105) 
REM   INTERNAL BONDS 
DISTANCES  0.0 , 0.01  = MEAN 
CONTINUE C(109) TO F(43) C(209) TO F(143) 
CONTINUE C(109) TO F(44) C(209) TO F(144) 
CONTINUE C(109) TO F(45) C(209) TO F(145) 
REM   ANGLES RESTRAINTS 
ANGLES  0.0 , 0.10  = MEAN 
CONTINUE F(43) TO C(109) TO C(105) F(143) TO C(209) TO C(105) 
CONTINUE F(44) TO C(109) TO C(105) F(144) TO C(209) TO C(105) 
CONTINUE F(44) TO C(109) TO F(43) F(144) TO C(209) TO F(143) 
CONTINUE F(45) TO C(109) TO C(105) F(145) TO C(209) TO C(105) 
CONTINUE F(45) TO C(109) TO F(43) F(145) TO C(209) TO F(143) 
CONTINUE F(45) TO C(109) TO F(44) F(145) TO C(209) TO F(144) 
REM   VIBRATIONAL RESTRAINTS 
VIBRATIONS 0.0, 0.0100  = 
CONTINUE C(109) TO C(105) C(209) TO C(105) 
CONTINUE C(109) TO F(43) C(209) TO F(143) 
CONTINUE C(109) TO F(44) C(209) TO F(144) 
CONTINUE C(109) TO F(45) C(209) TO F(145) 
VIBRATIONS 0.0, 0.00100  = 
CONTINUE C(109) TO C(209) 
CONTINUE F(43) TO F(143) 
CONTINUE F(44) TO F(144) 
CONTINUE F(45) TO F(145) 
REM   SIMILARITY RESTRAINTS 
U(IJ)'S 0.0, 0.0200  = 
CONTINUE C(109) TO C(105) C(209) TO C(105) 
CONTINUE C(109) TO F(43) C(209) TO F(143) 
CONTINUE C(109) TO F(44) C(209) TO F(144) 
CONTINUE C(109) TO F(45) C(209) TO F(145) 
U(IJ)'S 0.0, 0.00200  = 
CONTINUE C(109) TO C(209) 
CONTINUE F(43) TO F(143) 
CONTINUE F(44) TO F(144) 
CONTINUE F(45) TO F(145) 
REM   ASSEMBLY3   END (DO NOT REMOVE THIS LINE) 
REM   ASSEMBLY4   START (DO NOT REMOVE THIS LINE) 
REM   INTERNAL BONDS 
DISTANCES  1.75 , 0.01  = 
CONTINUE C(113) TO CL(5) C(213) TO CL(105) 
CONTINUE C(113) TO CL(6) C(213) TO CL(106) 
REM   ANGLES RESTRAINTS 
ANGLES  109.5 , 0.10  = 
CONTINUE CL(6) TO C(113) TO CL(5) CL(106) TO C(213) TO CL(105) 
REM   VIBRATIONAL RESTRAINTS 
VIBRATIONS 0.0, 0.00100  = 
CONTINUE C(113) TO CL(5) C(213) TO CL(105) 
CONTINUE C(113) TO CL(6) C(213) TO CL(106) 
VIBRATIONS 0.0, 0.0100  = 
CONTINUE C(113) TO C(213) 
CONTINUE CL(5) TO CL(105) 
CONTINUE CL(6) TO CL(106) 
REM   SIMILARITY RESTRAINTS 
U(IJ)'S 0.0, 0.0200  = 
CONTINUE C(113) TO CL(5) C(213) TO CL(105) 
CONTINUE C(113) TO CL(6) C(213) TO CL(106) 
U(IJ)'S 0.0, 0.00200  = 
CONTINUE C(113) TO C(213) 
CONTINUE CL(5) TO CL(105) 
CONTINUE CL(6) TO CL(106) 
REM   ASSEMBLY4   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;