Mechanistic studies of the dehydrocoupling and dehydropolymerization of amine-boranes using a [rh(xantphos)](+) catalyst.
Johnson, Heather C.; Leitao, Erin M.; Whittell, George R.; Manners, Ian; Lloyd-Jones, Guy C; Weller, Andrew S.; Journal of the American Chemical Society 136 (2014) 9078–9093; doi:10.1021/ja503335g

data_4122000
_publ_section_title
;
 Mechanistic studies of the dehydrocoupling and dehydropolymerization of
 amine-boranes using a [rh(xantphos)](+) catalyst.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9078
_journal_page_last               9093
_journal_paper_doi               10.1021/ja503335g
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C32 H12 B F24, C47 H51 B N2 O P2 Rh'
_chemical_formula_sum            'C79 H63 B2 F24 N2 O P2 Rh'
_chemical_formula_weight         1698.81
_chemical_name_systematic        '[Rh(XantPhos)(H)(BHNiPr2)(MeCN)][BArF4]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             13-11-05
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 94.9953(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.86840(10)
_cell_length_b                   14.9780(2)
_cell_length_c                   39.1771(3)
_cell_measurement_reflns_used    34352
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     8106.99(14)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34352
_diffrn_reflns_theta_full        74.824
_diffrn_reflns_theta_max         76.351
_diffrn_reflns_theta_min         3.160
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.955
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_platon_squeeze_details
;
;
_refine_diff_density_max         1.13
_refine_diff_density_min         -0.90
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1140
_refine_ls_number_reflns         16827
_refine_ls_number_restraints     1020
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.0187003
_refine_ls_shift/su_mean         0.0006113
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ +13.78P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1093
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1093
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              48
_reflns_limit_l_min              0
_reflns_number_gt                14814
_reflns_number_total             16891
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.08
_oxford_diffrn_Wilson_scale      0.68
_oxford_refine_ls_r_factor_ref   0.0516
_oxford_refine_ls_scale          1.310(3)
_oxford_reflns_number_all        16827
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title
'E:\Weller\hcj_013\CRYSTALS\hcj_0 At 17:59 on'
_cod_data_source_file            ja503335g_si_001.cif
_cod_data_source_block           10c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4122000.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C79 H63 B2 F24 N2 O1 P2 Rh1'
_cod_database_code               4122000
_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) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  23,X'S) H   (  21,X'S) H   (  22,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) 
RIDE C   (   5,X'S) H   (  52,X'S) H   (  51,X'S) H   (  53,X'S) 
RIDE C   (   6,X'S) H   (  63,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,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   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 161,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   (  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) 
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   (  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) 
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) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,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) 
RIDE RH  (   1,X'S) H   (   1,X'S) 
RIDE B   (   1,X'S) H   (   2,X'S) 
RIDE C   ( 280,X'S) H   (2802,X'S) H   (2801,X'S) H   (2803,X'S) 
RIDE C   ( 281,X'S) H   (2811,X'S) H   (2812,X'S) H   (2813,X'S) 
RIDE C   ( 290,X'S) H   (2901,X'S) H   (2902,X'S) H   (2903,X'S) 
RIDE C   ( 291,X'S) H   (2911,X'S) H   (2913,X'S) H   (2912,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(64) C(67) F(140) F(131) F(151) AND 
CONT C(64) C(67) F(131) F(151) F(140) AND 
CONT C(64) C(67) F(151) F(140) F(131) AND 
CONT C(64) C(67) F(141) F(130) F(150) AND 
CONT C(64) C(67) F(130) F(150) F(141) AND 
CONT C(64) C(67) F(150) F(141) F(130) 
DELU 0.015 C(64) C(67) F(140) F(131) F(151) AND 
CONT C(64) C(67) F(131) F(151) F(140) AND 
CONT C(64) C(67) F(151) F(140) F(131) AND 
CONT C(64) C(67) F(141) F(130) F(150) AND 
CONT C(64) C(67) F(130) F(150) F(141) AND 
CONT C(64) C(67) F(150) F(141) F(130) 
SIMU 0.015 C(64) C(67) F(140) F(131) F(151) AND 
CONT C(64) C(67) F(131) F(151) F(140) AND 
CONT C(64) C(67) F(151) F(140) F(131) AND 
CONT C(64) C(67) F(141) F(130) F(150) AND 
CONT C(64) C(67) F(130) F(150) F(141) AND 
CONT C(64) C(67) F(150) F(141) F(130) 
SAME C(72) C(75) F(211) F(201) F(190) AND 
CONT C(72) C(75) F(201) F(190) F(211) AND 
CONT C(72) C(75) F(190) F(211) F(201) AND 
CONT C(72) C(75) F(210) F(200) F(191) AND 
CONT C(72) C(75) F(200) F(191) F(210) AND 
CONT C(72) C(75) F(191) F(210) F(200) 
DELU 0.015 C(72) C(75) F(211) F(201) F(190) AND 
CONT C(72) C(75) F(201) F(190) F(211) AND 
CONT C(72) C(75) F(190) F(211) F(201) AND 
CONT C(72) C(75) F(210) F(200) F(191) AND 
CONT C(72) C(75) F(200) F(191) F(210) AND 
CONT C(72) C(75) F(191) F(210) F(200) 
SIMU 0.015 C(72) C(75) F(211) F(201) F(190) AND 
CONT C(72) C(75) F(201) F(190) F(211) AND 
CONT C(72) C(75) F(190) F(211) F(201) AND 
CONT C(72) C(75) F(210) F(200) F(191) AND 
CONT C(72) C(75) F(200) F(191) F(210) AND 
CONT C(72) C(75) F(191) F(210) F(200) 
SAME C(70) C(74) F(181) F(160) F(170) AND 
CONT C(70) C(74) F(160) F(170) F(181) AND 
CONT C(70) C(74) F(170) F(181) F(160) AND 
CONT C(70) C(74) F(180) F(161) F(171) AND 
CONT C(70) C(74) F(161) F(171) F(180) AND 
CONT C(70) C(74) F(171) F(180) F(161) 
DELU 0.015 C(70) C(74) F(181) F(160) F(170) AND 
CONT C(70) C(74) F(160) F(170) F(181) AND 
CONT C(70) C(74) F(170) F(181) F(160) AND 
CONT C(70) C(74) F(180) F(161) F(171) AND 
CONT C(70) C(74) F(161) F(171) F(180) AND 
CONT C(70) C(74) F(171) F(180) F(161) 
SIMU 0.015 C(70) C(74) F(181) F(160) F(170) AND 
CONT C(70) C(74) F(160) F(170) F(181) AND 
CONT C(70) C(74) F(170) F(181) F(160) AND 
CONT C(70) C(74) F(180) F(161) F(171) AND 
CONT C(70) C(74) F(161) F(171) F(180) AND 
CONT C(70) C(74) F(171) F(180) F(161) 
SAME C(62) C(66) F(111) F(100) F(120) AND 
CONT C(62) C(66) F(100) F(120) F(111) AND 
CONT C(62) C(66) F(120) F(111) F(100) AND 
CONT C(62) C(66) F(110) F(101) F(121) AND 
CONT C(62) C(66) F(101) F(121) F(110) AND 
CONT C(62) C(66) F(121) F(110) F(101) 
DELU 0.015 C(62) C(66) F(111) F(100) F(120) AND 
CONT C(62) C(66) F(100) F(120) F(111) AND 
CONT C(62) C(66) F(120) F(111) F(100) AND 
CONT C(62) C(66) F(110) F(101) F(121) AND 
CONT C(62) C(66) F(101) F(121) F(110) AND 
CONT C(62) C(66) F(121) F(110) F(101) 
SIMU 0.015 C(62) C(66) F(111) F(100) F(120) AND 
CONT C(62) C(66) F(100) F(120) F(111) AND 
CONT C(62) C(66) F(120) F(111) F(100) AND 
CONT C(62) C(66) F(110) F(101) F(121) AND 
CONT C(62) C(66) F(101) F(121) F(110) AND 
CONT C(62) C(66) F(121) F(110) F(101) 
SAME C(31) C(270) C(280) C(290)  AND 
CONT C(31) C(270) C(290) C(280)  AND 
CONT C(31) C(271) C(281) C(291)  AND 
CONT C(31) C(271) C(291) C(281) 
DELU 0.02 C(31) C(270) C(280) C(290)  AND 
CONT C(31) C(270) C(290) C(280)  AND 
CONT C(31) C(271) C(281) C(291)  AND 
CONT C(31) C(271) C(291) C(281) 
SIMU 0.02 C(31) C(270) C(280) C(290)  AND 
CONT C(31) C(270) C(290) C(280)  AND 
CONT C(31) C(271) C(281) C(291)  AND 
CONT C(31) C(271) C(291) C(281) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;