Dehydropolymerization of H3B·NMeH2 To Form Polyaminoboranes Using [Rh(Xantphos-alkyl)] Catalysts.
Adams, Gemma M.; Colebatch, Annie L.; Skornia, Joseph T.; McKay, Alasdair I.; Johnson, Heather C.; Lloyd Jones, Guy C.; Macgregor, Stuart A.; Beattie, Nicholas A.; Weller, Andrew S.; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b11975

data_4127064
_publ_section_title
;
 Dehydropolymerization of H3B&#x00B7;NMeH2 To Form Polyaminoboranes Using
 [Rh(Xantphos-alkyl)] Catalysts.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b11975
_journal_year                    2018
_chemical_formula_moiety         'C32 H12 B F24, C34 H48 O P2 Rh'
_chemical_formula_sum            'C66 H60 B F24 O P2 Rh'
_chemical_formula_weight         1500.82
_chemical_name_systematic        '[Rh(iPrXant)(nbd)][BArF4]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2015-06-22
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                90
_cell_angle_beta                 106.5796(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.8626(2)
_cell_length_b                   25.0729(2)
_cell_length_c                   24.0283(2)
_cell_measurement_reflns_used    26707
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     13201.1(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.983
_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  0.036
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            79001
_diffrn_reflns_theta_full        72.353
_diffrn_reflns_theta_max         76.161
_diffrn_reflns_theta_min         3.793
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.535
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6080
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.49
_refine_diff_density_min         -1.08
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9798
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1823
_refine_ls_number_reflns         27057
_refine_ls_number_restraints     912
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.0431569
_refine_ls_shift/su_mean         0.0003847
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +15.94P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1222
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1221
_reflns_limit_h_max              27
_reflns_limit_h_min              -28
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                22184
_reflns_number_total             27165
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.57
_oxford_diffrn_Wilson_scale      0.93
_oxford_refine_ls_r_factor_ref   0.0572
_oxford_refine_ls_scale          1.107(2)
_oxford_reflns_number_all        27060
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'C:\Was on D\Crystallography\HCJ_ At 10:51 on'
_iucr_refine_instructions_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) 
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) 
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   (   7,X'S) H   (  71,X'S) H   (  72,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  92,X'S) H   (  91,X'S) H   (  93,X'S) 
RIDE C   (  10,X'S) H   ( 102,X'S) H   ( 101,X'S) H   ( 103,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 123,X'S) H   ( 122,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 133,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 153,X'S) H   ( 152,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 163,X'S) H   ( 162,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 183,X'S) H   ( 182,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 193,X'S) H   ( 192,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   (  27,X'S) H   ( 272,X'S) H   ( 271,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 282,X'S) H   ( 281,X'S) H   ( 283,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   (  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   ( 412,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 423,X'S) H   ( 422,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 443,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 453,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   ( 473,X'S) H   ( 472,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 493,X'S) H   ( 492,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) H   ( 503,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 523,X'S) H   ( 522,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) H   ( 533,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  61,X'S) H   ( 612,X'S) H   ( 611,X'S) H   ( 613,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 623,X'S) H   ( 622,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  86,X'S) H   ( 861,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) 
RIDE C   (  94,X'S) H   ( 941,X'S) 
RIDE C   (  96,X'S) H   ( 961,X'S) 
RIDE C   (  98,X'S) H   ( 981,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 120,X'S) H   (1201,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) 
RIDE C   ( 126,X'S) H   (1261,X'S) 
RIDE C   ( 128,X'S) H   (1281,X'S) 
RIDE C   ( 130,X'S) H   (1301,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(121) C(124) F(501) F(511) F(520) AND 
CONT C(121) C(124) F(511) F(520) F(501) AND 
CONT C(121) C(124) F(520) F(501) F(511) AND 
CONT C(121) C(124) F(500) F(510) F(521) AND 
CONT C(121) C(124) F(510) F(521) F(500) AND 
CONT C(121) C(124) F(521) F(500) F(510) 
DELU 0.015 C(121) C(124) F(501) F(511) F(520) AND 
CONT C(121) C(124) F(511) F(520) F(501) AND 
CONT C(121) C(124) F(520) F(501) F(511) AND 
CONT C(121) C(124) F(500) F(510) F(521) AND 
CONT C(121) C(124) F(510) F(521) F(500) AND 
CONT C(121) C(124) F(521) F(500) F(510) 
SIMU 0.015 C(121) C(124) F(501) F(511) F(520) AND 
CONT C(121) C(124) F(511) F(520) F(501) AND 
CONT C(121) C(124) F(520) F(501) F(511) AND 
CONT C(121) C(124) F(500) F(510) F(521) AND 
CONT C(121) C(124) F(510) F(521) F(500) AND 
CONT C(121) C(124) F(521) F(500) F(510) 
SAME C(79) C(83) F(170) F(181) F(190) AND 
CONT C(79) C(83) F(181) F(190) F(170) AND 
CONT C(79) C(83) F(190) F(170) F(181) AND 
CONT C(79) C(83) F(171) F(180) F(191) AND 
CONT C(79) C(83) F(180) F(191) F(171) AND 
CONT C(79) C(83) F(191) F(171) F(180) 
DELU 0.015 C(79) C(83) F(170) F(181) F(190) AND 
CONT C(79) C(83) F(181) F(190) F(170) AND 
CONT C(79) C(83) F(190) F(170) F(181) AND 
CONT C(79) C(83) F(171) F(180) F(191) AND 
CONT C(79) C(83) F(180) F(191) F(171) AND 
CONT C(79) C(83) F(191) F(171) F(180) 
SIMU 0.015 C(79) C(83) F(170) F(181) F(190) AND 
CONT C(79) C(83) F(181) F(190) F(170) AND 
CONT C(79) C(83) F(190) F(170) F(181) AND 
CONT C(79) C(83) F(171) F(180) F(191) AND 
CONT C(79) C(83) F(180) F(191) F(171) AND 
CONT C(79) C(83) F(191) F(171) F(180) 
SAME C(87) C(91) F(230) F(240) F(251) AND 
CONT C(87) C(91) F(240) F(251) F(230) AND 
CONT C(87) C(91) F(251) F(230) F(240) AND 
CONT C(87) C(91) F(231) F(241) F(250) AND 
CONT C(87) C(91) F(241) F(250) F(231) AND 
CONT C(87) C(91) F(250) F(231) F(241) 
DELU 0.015 C(87) C(91) F(230) F(240) F(251) AND 
CONT C(87) C(91) F(240) F(251) F(230) AND 
CONT C(87) C(91) F(251) F(230) F(240) AND 
CONT C(87) C(91) F(231) F(241) F(250) AND 
CONT C(87) C(91) F(241) F(250) F(231) AND 
CONT C(87) C(91) F(250) F(231) F(241) 
SIMU 0.015 C(87) C(91) F(230) F(240) F(251) AND 
CONT C(87) C(91) F(240) F(251) F(230) AND 
CONT C(87) C(91) F(251) F(230) F(240) AND 
CONT C(87) C(91) F(231) F(241) F(250) AND 
CONT C(87) C(91) F(241) F(250) F(231) AND 
CONT C(87) C(91) F(250) F(231) F(241) 
SAME C(89) C(92) F(260) F(270) F(281) AND 
CONT C(89) C(92) F(270) F(281) F(260) AND 
CONT C(89) C(92) F(281) F(260) F(270) AND 
CONT C(89) C(92) F(261) F(271) F(280) AND 
CONT C(89) C(92) F(271) F(280) F(261) AND 
CONT C(89) C(92) F(280) F(261) F(271) 
DELU 0.015 C(89) C(92) F(260) F(270) F(281) AND 
CONT C(89) C(92) F(270) F(281) F(260) AND 
CONT C(89) C(92) F(281) F(260) F(270) AND 
CONT C(89) C(92) F(261) F(271) F(280) AND 
CONT C(89) C(92) F(271) F(280) F(261) AND 
CONT C(89) C(92) F(280) F(261) F(271) 
SIMU 0.015 C(89) C(92) F(260) F(270) F(281) AND 
CONT C(89) C(92) F(270) F(281) F(260) AND 
CONT C(89) C(92) F(281) F(260) F(270) AND 
CONT C(89) C(92) F(261) F(271) F(280) AND 
CONT C(89) C(92) F(271) F(280) F(261) AND 
CONT C(89) C(92) F(280) F(261) F(271) 
END                                                                             
;
_cod_data_source_file            ja7b11975_si_002.cif
_cod_data_source_block           complex_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C66 H60 B1 F24 O1 P2 Rh1'
_cod_database_code               4127064