Exploring the mechanism of the hydroboration of alkenes by amine‒boranes catalysed by [Rh(xantphos)]+
Johnson, Heather C.; Torry-Harris, Rebecca; Ortega, Laura; Theron, Robin; McIndoe, J. Scott; Weller, Andrew S.; Catal. Sci. Technol. 4 (2014) 3486–; doi:10.1039/C4CY00597J

data_1517894
_publ_section_title
;
 Exploring the mechanism of the hydroboration of alkenes by amine--boranes
 catalysed by [Rh(xantphos)]+
;
_journal_issue                   10
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              3486
_journal_paper_doi               10.1039/C4CY00597J
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C47 H56 B1 N1 O1 P2 Rh1 Si1, C32 H12 B1 F24'
_chemical_formula_sum            'C79 H68 B2 F24 N O P2 Rh Si'
_chemical_formula_weight         1717.93
_chemical_name_systematic        '[Rh(XantPhos)(H2BCH2CH2SiME3NMe3)][BArF4]'
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             14-03-28
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                110.6501(11)
_cell_angle_beta                 107.1873(12)
_cell_angle_gamma                106.290(2)
_cell_formula_units_Z            2
_cell_length_a                   16.6243(5)
_cell_length_b                   16.8939(5)
_cell_length_c                   17.7667(7)
_cell_measurement_reflns_used    12902
_cell_measurement_temperature    150
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     4026.5(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.078
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            36954
_diffrn_reflns_theta_full        25.018
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_min         5.113
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.9327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1744.000
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
;
_refine_diff_density_max         3.32
_refine_diff_density_min         -1.68
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9482
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1186
_refine_ls_number_reflns         11566
_refine_ls_number_restraints     2846
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0860
_refine_ls_shift/su_max          0.0476194
_refine_ls_shift/su_mean         0.0006242
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ +27.29P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2043
_refine_ls_wR_factor_gt          0.1973
_refine_ls_wR_factor_ref         0.2043
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              18
_reflns_limit_k_min              -20
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                8864
_reflns_number_total             14012
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.65
_oxford_diffrn_Wilson_scale      46.24
_oxford_refine_ls_r_factor_ref   0.1182
_oxford_refine_ls_scale          0.17630(12)
_oxford_reflns_number_all        11566
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'Compound X At 12:55 on 15/ 3'
_cod_duplicate_entry             1516575
_cod_data_source_file            c4cy00597j2.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C79 H68 B2 F24 N1 O1 P2 Rh1 Si1'
_cod_database_code               1517894
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIV PART(2001,OCC) PART(2002,OCC) 
WEIGHT -1 PART(2002,OCC) 
EQUIV PART(3001,OCC) PART(3002,OCC) 
WEIGHT -1 PART(3002,OCC) 
EQUIV PART(4001,OCC) PART(4002,OCC) 
WEIGHT -1 PART(4002,OCC) 
EQUIV PART(5001,OCC) PART(5002,OCC) 
WEIGHT -1 PART(5002,OCC) 
EQUIV PART(6001,OCC) PART(6002,OCC) 
WEIGHT -1 PART(6002,OCC) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  98,X'S) H   ( 981,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (  79,X'S) H   ( 791,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  20,X'S) H   ( 203,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 213,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) 
RIDE C   ( 128,X'S) H   (1281,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  93,X'S) H   ( 931,X'S) H   ( 932,X'S) 
RIDE B   (   1,X'S) H   (  12,X'S) H   (  11,X'S) 
RIDE C   ( 126,X'S) H   (1262,X'S) H   (1261,X'S) H   (1263,X'S) 
RIDE C   (  96,X'S) H   ( 961,X'S) H   ( 962,X'S) H   ( 963,X'S) 
RIDE C   ( 910,X'S) H   (9101,X'S) H   (9103,X'S) H   (9102,X'S) 
RIDE C   ( 911,X'S) H   (9112,X'S) H   (9111,X'S) H   (9113,X'S) 
RIDE C   ( 920,X'S) H   (9201,X'S) H   (9202,X'S) H   (9203,X'S) 
RIDE C   ( 921,X'S) H   (9211,X'S) H   (9213,X'S) H   (9212,X'S) 
RIDE C   ( 900,X'S) H   (9003,X'S) H   (9001,X'S) H   (9002,X'S) 
RIDE C   ( 901,X'S) H   (9011,X'S) H   (9013,X'S) H   (9012,X'S) 
RIDE C   ( 940,X'S) H   (9401,X'S) H   (9402,X'S) 
RIDE C   ( 941,X'S) H   (9411,X'S) H   (9412,X'S) 
RIDE C   ( 970,X'S) H   (9701,X'S) H   (9703,X'S) H   (9702,X'S) 
RIDE C   ( 971,X'S) H   (9712,X'S) H   (9711,X'S) H   (9713,X'S) 
RIDE C   ( 950,X'S) H   (9501,X'S) H   (9502,X'S) H   (9503,X'S) 
RIDE C   ( 951,X'S) H   (9511,X'S) H   (9513,X'S) H   (9512,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(60) C(64) F(341) F(350) F(120) AND 
CONT C(60) C(64) F(350) F(120) F(341) AND 
CONT C(60) C(64) F(120) F(341) F(350) AND 
CONT C(60) C(64) F(340) F(351) F(121) AND 
CONT C(60) C(64) F(351) F(121) F(340) AND 
CONT C(60) C(64) F(121) F(340) F(351) 
DELU 0.015 C(60) C(64) F(341) F(350) F(120) AND 
CONT C(60) C(64) F(350) F(120) F(341) AND 
CONT C(60) C(64) F(120) F(341) F(350) AND 
CONT C(60) C(64) F(340) F(351) F(121) AND 
CONT C(60) C(64) F(351) F(121) F(340) AND 
CONT C(60) C(64) F(121) F(340) F(351) 
SIMU 0.015 C(60) C(64) F(341) F(350) F(120) AND 
CONT C(60) C(64) F(350) F(120) F(341) AND 
CONT C(60) C(64) F(120) F(341) F(350) AND 
CONT C(60) C(64) F(340) F(351) F(121) AND 
CONT C(60) C(64) F(351) F(121) F(340) AND 
CONT C(60) C(64) F(121) F(340) F(351) 
SAME C(62) C(65) F(180) F(1010) F(171) AND 
CONT C(62) C(65) F(1010) F(171) F(180) AND 
CONT C(62) C(65) F(171) F(180) F(1010) AND 
CONT C(62) C(65) F(181) F(1011) F(170) AND 
CONT C(62) C(65) F(1011) F(170) F(181) AND 
CONT C(62) C(65) F(170) F(181) F(1011) 
DELU 0.015 C(62) C(65) F(180) F(1010) F(171) AND 
CONT C(62) C(65) F(1010) F(171) F(180) AND 
CONT C(62) C(65) F(171) F(180) F(1010) AND 
CONT C(62) C(65) F(181) F(1011) F(170) AND 
CONT C(62) C(65) F(1011) F(170) F(181) AND 
CONT C(62) C(65) F(170) F(181) F(1011) 
SIMU 0.015 C(62) C(65) F(180) F(1010) F(171) AND 
CONT C(62) C(65) F(1010) F(171) F(180) AND 
CONT C(62) C(65) F(171) F(180) F(1010) AND 
CONT C(62) C(65) F(181) F(1011) F(170) AND 
CONT C(62) C(65) F(1011) F(170) F(181) AND 
CONT C(62) C(65) F(170) F(181) F(1011) 
SAME C(54) C(57) F(110) F(861) F(870) AND 
CONT C(54) C(57) F(861) F(870) F(110) AND 
CONT C(54) C(57) F(870) F(110) F(861) AND 
CONT C(54) C(57) F(111) F(860) F(871) AND 
CONT C(54) C(57) F(860) F(871) F(111) AND 
CONT C(54) C(57) F(871) F(111) F(860) 
DELU 0.015 C(54) C(57) F(110) F(861) F(870) AND 
CONT C(54) C(57) F(861) F(870) F(110) AND 
CONT C(54) C(57) F(870) F(110) F(861) AND 
CONT C(54) C(57) F(111) F(860) F(871) AND 
CONT C(54) C(57) F(860) F(871) F(111) AND 
CONT C(54) C(57) F(871) F(111) F(860) 
SIMU 0.015 C(54) C(57) F(110) F(861) F(870) AND 
CONT C(54) C(57) F(861) F(870) F(110) AND 
CONT C(54) C(57) F(870) F(110) F(861) AND 
CONT C(54) C(57) F(111) F(860) F(871) AND 
CONT C(54) C(57) F(860) F(871) F(111) AND 
CONT C(54) C(57) F(871) F(111) F(860) 
SAME C(52) C(56) F(201) F(161) F(240) AND 
CONT C(52) C(56) F(161) F(240) F(201) AND 
CONT C(52) C(56) F(240) F(201) F(161) AND 
CONT C(52) C(56) F(200) F(160) F(241) AND 
CONT C(52) C(56) F(160) F(241) F(200) AND 
CONT C(52) C(56) F(241) F(200) F(160) 
DELU 0.015 C(52) C(56) F(201) F(161) F(240) AND 
CONT C(52) C(56) F(161) F(240) F(201) AND 
CONT C(52) C(56) F(240) F(201) F(161) AND 
CONT C(52) C(56) F(200) F(160) F(241) AND 
CONT C(52) C(56) F(160) F(241) F(200) AND 
CONT C(52) C(56) F(241) F(200) F(160) 
SIMU 0.015 C(52) C(56) F(201) F(161) F(240) AND 
CONT C(52) C(56) F(161) F(240) F(201) AND 
CONT C(52) C(56) F(240) F(201) F(161) AND 
CONT C(52) C(56) F(200) F(160) F(241) AND 
CONT C(52) C(56) F(160) F(241) F(200) AND 
CONT C(52) C(56) F(241) F(200) F(160) 
SAME B(1) N(1) C(900) C(911) C(921) AND 
CONT B(1) N(1) C(911) C(921) C(900) AND 
CONT B(1) N(1) C(921) C(900) C(911) AND 
CONT B(1) N(1) C(901) C(910) C(920) AND 
CONT B(1) N(1) C(910) C(920) C(901) AND 
CONT B(1) N(1) C(920) C(901) C(910) 
DELU 0.015 B(1) N(1) C(900) C(911) C(921) AND 
CONT B(1) N(1) C(911) C(921) C(900) AND 
CONT B(1) N(1) C(921) C(900) C(911) AND 
CONT B(1) N(1) C(901) C(910) C(920) AND 
CONT B(1) N(1) C(910) C(920) C(901) AND 
CONT B(1) N(1) C(920) C(901) C(910) 
SIMU 0.015 B(1) N(1) C(900) C(911) C(921) AND 
CONT B(1) N(1) C(911) C(921) C(900) AND 
CONT B(1) N(1) C(921) C(900) C(911) AND 
CONT B(1) N(1) C(901) C(910) C(920) AND 
CONT B(1) N(1) C(910) C(920) C(901) AND 
CONT B(1) N(1) C(920) C(901) C(910) 
SAME C(93) C(940) SI(1) C(971) AND 
CONT C(93) C(941) SI(2) C(970) 
DELU 0.015 C(93) C(940) SI(1) C(971) AND 
CONT C(93) C(941) SI(2) C(970) 
SIMU 0.015 C(93) C(940) SI(1) C(971) AND 
CONT C(93) C(941) SI(2) C(970) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
LIMIT      0.01000000 U[ISO] 
LIMIT      0.01000000 X 
LIMIT      0.01000000 Y 
LIMIT      0.01000000 Z 
LIMIT      0.01000000 U[11] 
LIMIT      0.01000000 U[22] 
LIMIT      0.01000000 U[33] 
LIMIT      0.01000000 U[12] 
LIMIT      0.01000000 U[13] 
LIMIT      0.01000000 U[23] 
LIMIT      0.01000000 OCC 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;