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_4127063
_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_compound_source        SYN
_chemical_formula_moiety         'C32 H12 B1 F24, C30 H40 O1 P2 Rh1'
_chemical_formula_sum            'C62 H52 B F24 O P2 Rh'
_chemical_formula_weight         1444.71
_chemical_melting_point          ?
_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     direct
_audit_creation_date             2016-11-14
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                90
_cell_angle_beta                 102.1591(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6622(2)
_cell_length_b                   17.9481(2)
_cell_length_c                   19.1933(3)
_cell_measurement_reflns_used    16325
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     6284.59(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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38228
_diffrn_reflns_theta_full        74.060
_diffrn_reflns_theta_max         76.351
_diffrn_reflns_theta_min         3.884
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.689
_exptl_absorpt_correction_T_max  0.48
_exptl_absorpt_correction_T_min  0.39
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.13
_refine_diff_density_min         -1.64
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9583
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1014
_refine_ls_number_reflns         12965
_refine_ls_number_restraints     1596
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.0063564
_refine_ls_shift/su_mean         0.0000813
_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: 
 0.320E+04 0.534E+04 0.324E+04 0.134E+04 296. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1601
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1601
_reflns_limit_h_max              22
_reflns_limit_h_min              -23
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                11509
_reflns_number_total             13014
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.39
_oxford_diffrn_Wilson_scale      0.18
_oxford_refine_ls_r_factor_ref   0.0676
_oxford_refine_ls_scale          2.66(2)
_oxford_reflns_number_all        12966
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'C:\Users\aswgroup\Desktop\Crysta At 9:56 on '
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'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   (   8,X'S) H   (  81,X'S) H   (  83,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  93,X'S) H   (  92,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   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 172,X'S) H   ( 171,X'S) H   ( 173,X'S) 
RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 193,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) H   ( 213,X'S) 
RIDE C   (  22,X'S) H   ( 222,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 233,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIV PART(3001,OCC) PART(3002,OCC) 
WEIGHT -1 PART(3002,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) 
EQUIV PART(7001,OCC) PART(7002,OCC) 
WEIGHT -1 PART(7002,OCC) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(33) C(37) F(310) F(320) F(330) AND 
CONT C(33) C(37) F(320) F(330) F(310) AND 
CONT C(33) C(37) F(330) F(310) F(320) AND 
CONT C(33) C(37) F(311) F(321) F(331) AND 
CONT C(33) C(37) F(321) F(331) F(311) AND 
CONT C(33) C(37) F(331) F(311) F(321) 
DELU 0.015 C(33) C(37) F(310) F(320) F(330) AND 
CONT C(33) C(37) F(320) F(330) F(310) AND 
CONT C(33) C(37) F(330) F(310) F(320) AND 
CONT C(33) C(37) F(311) F(321) F(331) AND 
CONT C(33) C(37) F(321) F(331) F(311) AND 
CONT C(33) C(37) F(331) F(311) F(321) 
SIMU 0.015 C(33) C(37) F(310) F(320) F(330) AND 
CONT C(33) C(37) F(320) F(330) F(310) AND 
CONT C(33) C(37) F(330) F(310) F(320) AND 
CONT C(33) C(37) F(311) F(321) F(331) AND 
CONT C(33) C(37) F(321) F(331) F(311) AND 
CONT C(33) C(37) F(331) F(311) F(321) 
SAME C(35) C(38) F(40) F(50) F(60) AND 
CONT C(35) C(38) F(50) F(60) F(40) AND 
CONT C(35) C(38) F(60) F(40) F(50) AND 
CONT C(35) C(38) F(41) F(51) F(61) AND 
CONT C(35) C(38) F(51) F(61) F(41) AND 
CONT C(35) C(38) F(61) F(41) F(51) 
DELU 0.015 C(35) C(38) F(40) F(50) F(60) AND 
CONT C(35) C(38) F(50) F(60) F(40) AND 
CONT C(35) C(38) F(60) F(40) F(50) AND 
CONT C(35) C(38) F(41) F(51) F(61) AND 
CONT C(35) C(38) F(51) F(61) F(41) AND 
CONT C(35) C(38) F(61) F(41) F(51) 
SIMU 0.015 C(35) C(38) F(40) F(50) F(60) AND 
CONT C(35) C(38) F(50) F(60) F(40) AND 
CONT C(35) C(38) F(60) F(40) F(50) AND 
CONT C(35) C(38) F(41) F(51) F(61) AND 
CONT C(35) C(38) F(51) F(61) F(41) AND 
CONT C(35) C(38) F(61) F(41) F(51) 
SAME C(41) C(45) F(70) F(80) F(90) AND 
CONT C(41) C(45) F(80) F(90) F(70) AND 
CONT C(41) C(45) F(90) F(70) F(80) AND 
CONT C(41) C(45) F(71) F(81) F(91) AND 
CONT C(41) C(45) F(81) F(91) F(71) AND 
CONT C(41) C(45) F(91) F(71) F(81) 
DELU 0.015 C(41) C(45) F(70) F(80) F(90) AND 
CONT C(41) C(45) F(80) F(90) F(70) AND 
CONT C(41) C(45) F(90) F(70) F(80) AND 
CONT C(41) C(45) F(71) F(81) F(91) AND 
CONT C(41) C(45) F(81) F(91) F(71) AND 
CONT C(41) C(45) F(91) F(71) F(81) 
SIMU 0.015 C(41) C(45) F(70) F(80) F(90) AND 
CONT C(41) C(45) F(80) F(90) F(70) AND 
CONT C(41) C(45) F(90) F(70) F(80) AND 
CONT C(41) C(45) F(71) F(81) F(91) AND 
CONT C(41) C(45) F(81) F(91) F(71) AND 
CONT C(41) C(45) F(91) F(71) F(81) 
SAME C(43) C(46) F(100) F(110) F(120) AND 
CONT C(43) C(46) F(110) F(120) F(100) AND 
CONT C(43) C(46) F(120) F(100) F(110) AND 
CONT C(43) C(46) F(101) F(111) F(121) AND 
CONT C(43) C(46) F(111) F(121) F(101) AND 
CONT C(43) C(46) F(121) F(101) F(111) 
DELU 0.015 C(43) C(46) F(100) F(110) F(120) AND 
CONT C(43) C(46) F(110) F(120) F(100) AND 
CONT C(43) C(46) F(120) F(100) F(110) AND 
CONT C(43) C(46) F(101) F(111) F(121) AND 
CONT C(43) C(46) F(111) F(121) F(101) AND 
CONT C(43) C(46) F(121) F(101) F(111) 
SIMU 0.015 C(43) C(46) F(100) F(110) F(120) AND 
CONT C(43) C(46) F(110) F(120) F(100) AND 
CONT C(43) C(46) F(120) F(100) F(110) AND 
CONT C(43) C(46) F(101) F(111) F(121) AND 
CONT C(43) C(46) F(111) F(121) F(101) AND 
CONT C(43) C(46) F(121) F(101) F(111) 
SAME C(49) C(53) F(410) F(420) F(430) AND 
CONT C(49) C(53) F(420) F(430) F(410) AND 
CONT C(49) C(53) F(430) F(410) F(420) AND 
CONT C(49) C(53) F(411) F(421) F(431) AND 
CONT C(49) C(53) F(421) F(431) F(411) AND 
CONT C(49) C(53) F(431) F(411) F(421) 
DELU 0.015 C(49) C(53) F(410) F(420) F(430) AND 
CONT C(49) C(53) F(420) F(430) F(410) AND 
CONT C(49) C(53) F(430) F(410) F(420) AND 
CONT C(49) C(53) F(411) F(421) F(431) AND 
CONT C(49) C(53) F(421) F(431) F(411) AND 
CONT C(49) C(53) F(431) F(411) F(421) 
SIMU 0.015 C(49) C(53) F(410) F(420) F(430) AND 
CONT C(49) C(53) F(420) F(430) F(410) AND 
CONT C(49) C(53) F(430) F(410) F(420) AND 
CONT C(49) C(53) F(411) F(421) F(431) AND 
CONT C(49) C(53) F(421) F(431) F(411) AND 
CONT C(49) C(53) F(431) F(411) F(421) 
SAME C(57) C(61) F(510) F(521) F(531) AND 
CONT C(57) C(61) F(521) F(531) F(510) AND 
CONT C(57) C(61) F(531) F(510) F(521) AND 
CONT C(57) C(61) F(511) F(520) F(530) AND 
CONT C(57) C(61) F(520) F(530) F(511) AND 
CONT C(57) C(61) F(530) F(511) F(520) 
DELU 0.015 C(57) C(61) F(510) F(521) F(531) AND 
CONT C(57) C(61) F(521) F(531) F(510) AND 
CONT C(57) C(61) F(531) F(510) F(521) AND 
CONT C(57) C(61) F(511) F(520) F(530) AND 
CONT C(57) C(61) F(520) F(530) F(511) AND 
CONT C(57) C(61) F(530) F(511) F(520) 
SIMU 0.015 C(57) C(61) F(510) F(521) F(531) AND 
CONT C(57) C(61) F(521) F(531) F(510) AND 
CONT C(57) C(61) F(531) F(510) F(521) AND 
CONT C(57) C(61) F(511) F(520) F(530) AND 
CONT C(57) C(61) F(520) F(530) F(511) AND 
CONT C(57) C(61) F(530) F(511) F(520) 
SAME C(59) C(62) F(220) F(230) F(240) AND 
CONT C(59) C(62) F(230) F(240) F(220) AND 
CONT C(59) C(62) F(240) F(220) F(230) AND 
CONT C(59) C(62) F(221) F(231) F(241) AND 
CONT C(59) C(62) F(231) F(241) F(221) AND 
CONT C(59) C(62) F(241) F(221) F(231) 
DELU 0.015 C(59) C(62) F(220) F(230) F(240) AND 
CONT C(59) C(62) F(230) F(240) F(220) AND 
CONT C(59) C(62) F(240) F(220) F(230) AND 
CONT C(59) C(62) F(221) F(231) F(241) AND 
CONT C(59) C(62) F(231) F(241) F(221) AND 
CONT C(59) C(62) F(241) F(221) F(231) 
SIMU 0.015 C(59) C(62) F(220) F(230) F(240) AND 
CONT C(59) C(62) F(230) F(240) F(220) AND 
CONT C(59) C(62) F(240) F(220) F(230) AND 
CONT C(59) C(62) F(221) F(231) F(241) AND 
CONT C(59) C(62) F(231) F(241) F(221) AND 
CONT C(59) C(62) F(241) F(221) F(231) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_cod_data_source_file            ja7b11975_si_002.cif
_cod_data_source_block           complex_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C62 H52 B1 F24 O1 P2 Rh1'
_cod_database_code               4127063