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_1517895
_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         'C32 H12 B1 F24, C57 H65 O1 P3 Rh1'
_chemical_formula_sum            'C89 H77 B F24 O P3 Rh'
_chemical_formula_weight         1825.18
_chemical_name_systematic        '[Rh(Xantphos)(PCy3)][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             14-03-17
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                87.9991(5)
_cell_angle_beta                 74.6948(5)
_cell_angle_gamma                87.0039(6)
_cell_formula_units_Z            2
_cell_length_a                   12.90760(10)
_cell_length_b                   17.8030(2)
_cell_length_c                   19.9590(3)
_cell_measurement_reflns_used    17430
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4416.68(9)
_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 0.990
_diffrn_measured_fraction_theta_max 0.988
_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  0.050
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            61434
_diffrn_reflns_theta_full        25.292
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         5.099
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.9400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.130
_platon_squeeze_details
;
;
_refine_diff_density_max         1.18
_refine_diff_density_min         -0.85
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9426
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1128
_refine_ls_number_reflns         20022
_refine_ls_number_restraints     456
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.0430749
_refine_ls_shift/su_mean         0.0011332
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ + 1.57P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1393
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1393
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              23
_reflns_limit_k_min              -23
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                14530
_reflns_number_total             20022
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.80
_oxford_diffrn_Wilson_scale      32.10
_oxford_refine_ls_r_factor_ref   0.0857
_oxford_refine_ls_scale          0.19284(9)
_oxford_reflns_number_all        20022
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'HCJ_009 At 16:56 on 21/ 8'
_cod_duplicate_entry             1516576
_cod_data_source_file            c4cy00597j2.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C89 H77 B1 F24 O1 P3 Rh1'
_cod_database_code               1517895
_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) 
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   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,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   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) H   ( 203,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,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   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,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   (  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) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) H   ( 472,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 482,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) H   ( 492,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) H   ( 572,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) 
RIDE C   (  79,X'S) H   ( 791,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) 
RIDE C   (  87,X'S) H   ( 871,X'S) 
RIDE C   (  89,X'S) H   ( 891,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(88) C(90) F(221) F(240) F(231) AND 
CONT C(88) C(90) F(240) F(231) F(221) AND 
CONT C(88) C(90) F(231) F(221) F(240) AND 
CONT C(88) C(90) F(220) F(241) F(230) AND 
CONT C(88) C(90) F(241) F(230) F(220) AND 
CONT C(88) C(90) F(230) F(220) F(241) 
DELU 0.015 C(88) C(90) F(221) F(240) F(231) AND 
CONT C(88) C(90) F(240) F(231) F(221) AND 
CONT C(88) C(90) F(231) F(221) F(240) AND 
CONT C(88) C(90) F(220) F(241) F(230) AND 
CONT C(88) C(90) F(241) F(230) F(220) AND 
CONT C(88) C(90) F(230) F(220) F(241) 
SIMU 0.015 C(88) C(90) F(221) F(240) F(231) AND 
CONT C(88) C(90) F(240) F(231) F(221) AND 
CONT C(88) C(90) F(231) F(221) F(240) AND 
CONT C(88) C(90) F(220) F(241) F(230) AND 
CONT C(88) C(90) F(241) F(230) F(220) AND 
CONT C(88) C(90) F(230) F(220) F(241) 
SAME C(80) C(83) F(170) F(181) F(160) AND 
CONT C(80) C(83) F(181) F(160) F(170) AND 
CONT C(80) C(83) F(160) F(170) F(181) AND 
CONT C(80) C(83) F(171) F(180) F(161) AND 
CONT C(80) C(83) F(180) F(161) F(171) AND 
CONT C(80) C(83) F(161) F(171) F(180) 
DELU 0.015 C(80) C(83) F(170) F(181) F(160) AND 
CONT C(80) C(83) F(181) F(160) F(170) AND 
CONT C(80) C(83) F(160) F(170) F(181) AND 
CONT C(80) C(83) F(171) F(180) F(161) AND 
CONT C(80) C(83) F(180) F(161) F(171) AND 
CONT C(80) C(83) F(161) F(171) F(180) 
SIMU 0.015 C(80) C(83) F(170) F(181) F(160) AND 
CONT C(80) C(83) F(181) F(160) F(170) AND 
CONT C(80) C(83) F(160) F(170) F(181) AND 
CONT C(80) C(83) F(171) F(180) F(161) AND 
CONT C(80) C(83) F(180) F(161) F(171) AND 
CONT C(80) C(83) F(161) F(171) F(180) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;