Catching the First Oligomerization Event in the Catalytic Formation of Polyaminoboranes: H3B.NMeHBH2.NMeH2 Bound to Iridium
Heather C. Johnson; Alasdair P. M. Robertson; Adrian B. Chaplin; Laura J. Sewell; Amber L. Thompson; Mairi F. Haddow; Ian Manners; Andrew S. Weller; Journal of the American Chemical Society 133 (2011) 11076–11079; doi:10.1021/ja2040738

data_4106464
_publ_section_title
;
 Catching the First Oligomerization Event in the Catalytic Formation of
 Polyaminoboranes: H3B.NMeHBH2.NMeH2 Bound to Iridium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11076
_journal_page_last               11079
_journal_paper_doi               10.1021/ja2040738
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C67 H104 B3 Cl8 Ir1 N2 P2'
_chemical_formula_sum            'C67 H104 B3 Cl8 Ir N2 P2'
_chemical_formula_weight         1507.80
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_date             11-03-24
_audit_creation_method           CRYSTALS_ver_14.20
_cell_angle_alpha                72.626(13)
_cell_angle_beta                 74.181(10)
_cell_angle_gamma                69.118(12)
_cell_formula_units_Z            2
_cell_length_a                   13.418(3)
_cell_length_b                   14.765(3)
_cell_length_c                   23.308(6)
_cell_measurement_reflns_used    13625
_cell_measurement_temperature    150
_cell_measurement_theta_max      31
_cell_measurement_theta_min      0
_cell_volume                     4045.4(17)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_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      150
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_details
;
scan:
    Number of images: 175
               Slice: -60.0000 - 115.0000
         Image width: 1.0000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 0.0000
                 XTD: 60.1015
              2theta: 29.8090
scan:
    Number of images: 120
               Slice: -60.0000 - 60.0000
         Image width: 1.0000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -50.0000
                 Phi: 0.0000
                 XTD: 60.1015
              2theta: 29.8090
scan:
    Number of images: 120
               Slice: -60.0000 - 60.0000
         Image width: 1.0000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -50.0000
                 Phi: 120.0000
                 XTD: 60.1015
              2theta: 29.8090
scan:
    Number of images: 120
               Slice: -60.0000 - 60.0000
         Image width: 1.0000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -50.0000
                 Phi: 240.0000
                 XTD: 60.1015
              2theta: 29.8090

;
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle) CCD'
_diffrn_measurement_device_type  'Rigaku Saturn724+ CCD (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.007758
_diffrn_orient_matrix_UB_12      -0.007662
_diffrn_orient_matrix_UB_13      0.080451
_diffrn_orient_matrix_UB_21      0.065017
_diffrn_orient_matrix_UB_22      -0.019232
_diffrn_orient_matrix_UB_23      -0.030584
_diffrn_orient_matrix_UB_31      -0.000249
_diffrn_orient_matrix_UB_32      0.045558
_diffrn_orient_matrix_UB_33      -0.004241
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24583
_diffrn_reflns_theta_full        25.182
_diffrn_reflns_theta_max         31.478
_diffrn_reflns_theta_min         0.903
_diffrn_source                   Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.989
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_exptl_crystal_colour            clear_intense_yellow
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       plate
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure factors.
;
_refine_diff_density_max         1.40
_refine_diff_density_min         -2.69
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         24582
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.0043092
_refine_ls_shift/su_mean         0.0000261
_refine_ls_structure_factor_coef Fsqd
_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: 
 35.2 53.5 29.5 10.7 2.39 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1069
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1069
_reflns_limit_h_max              20
_reflns_limit_h_min              -19
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                21695
_reflns_number_total             24583
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.33
_oxford_diffrn_Wilson_scale      14.79
_oxford_refine_ls_r_factor_ref   0.0582
_oxford_refine_ls_scale          0.25672(8)
_oxford_reflns_number_all        24582
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title DIA0123
_cod_data_source_file            ja2040738_si_004.cif
_cod_data_source_block           DIA0123
_cod_original_cell_volume        4045.6(18)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C67 H104 B3 Cl8 Ir1 N2 P2'
_cod_database_code               4106464
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE IR  (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE B   (   1,X'S) H   (  13,X'S) H   (  14,X'S) H   (  15,X'S) 
RIDE N   (   1,X'S) H   (  16,X'S) 
RIDE C   (   1,X'S) H   (  17,X'S) H   (  18,X'S) H   (  19,X'S) 
RIDE B   (   2,X'S) H   (  20,X'S) H   (  21,X'S) 
RIDE N   (   2,X'S) H   (  22,X'S) H   (  23,X'S) 
RIDE C   (   2,X'S) H   (  24,X'S) H   (  25,X'S) H   (  26,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) H   (1012,X'S) H   (1013,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) H   (1022,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) H   (1032,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) H   (1042,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) H   (1052,X'S) H   (1053,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) 
END                                                                             
;