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_4127065
_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_absolute_configuration unk
_chemical_formula_moiety         'C32 H12 B F24, C30 H54 B N O P2 Rh'
_chemical_formula_sum            'C62 H66 B2 F24 N O P2 Rh'
_chemical_formula_weight         1483.64
_chemical_name_systematic        '[Rh(iPrXant)(H)2(H3BNMe3)][BArF4]'
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2015-06-24
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.32780(10)
_cell_length_b                   13.11580(10)
_cell_length_c                   26.1296(2)
_cell_measurement_reflns_used    44206
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     6623.84(8)
_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 0.996
_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  0.056
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            80376
_diffrn_reflns_theta_full        76.229
_diffrn_reflns_theta_max         76.229
_diffrn_reflns_theta_min         3.370
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.514
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.33
_refine_diff_density_min         -0.70
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9794
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         7048
_refine_ls_number_restraints     285
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.0398114
_refine_ls_shift/su_mean         0.0011377
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 7.75P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1049
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1048
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                6888
_reflns_number_total             7081
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.77
_oxford_diffrn_Wilson_scale      0.50
_oxford_refine_ls_r_factor_ref   0.0408
_oxford_refine_ls_scale          2.214(14)
_oxford_reflns_number_all        7050
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title
'C:\Was on D\Crystallography\HCJ_ At 9:10 on '
_cod_data_source_file            ja7b11975_si_002.cif
_cod_data_source_block           complex_6
_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 c a 21 '
_cod_original_formula_sum        'C62 H66 B2 F24 N1 O1 P2 Rh1'
_cod_database_code               4127065
_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) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  13,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  22,X'S) H   (  21,X'S) H   (  23,X'S) 
RIDE C   (   3,X'S) H   (  32,X'S) H   (  33,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  43,X'S) H   (  42,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  63,X'S) H   (  62,X'S) 
RIDE C   (   7,X'S) H   (  72,X'S) H   (  71,X'S) H   (  73,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  92,X'S) H   (  93,X'S) H   (  91,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   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) H   ( 173,X'S) 
RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 183,X'S) H   ( 181,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 302,X'S) H   ( 303,X'S) H   ( 301,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE RH  (   1,X'S) H   (   1,X'S) H   (   2,X'S) 
RIDE B   (   1,X'S) H   (   5,X'S) H   (   3,X'S) H   (   4,X'S) 
RIDE C   ( 250,X'S) H   (2501,X'S) 
RIDE C   ( 251,X'S) H   (2511,X'S) 
RIDE C   ( 270,X'S) H   (2702,X'S) H   (2703,X'S) H   (2701,X'S) 
RIDE C   ( 271,X'S) H   (2711,X'S) H   (2712,X'S) H   (2713,X'S) 
RIDE C   ( 260,X'S) H   (2601,X'S) H   (2602,X'S) H   (2603,X'S) 
RIDE C   ( 261,X'S) H   (2612,X'S) H   (2613,X'S) H   (2611,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(68) C(71) F(220) F(240) F(231) AND 
CONT C(68) C(71) F(240) F(231) F(220) AND 
CONT C(68) C(71) F(231) F(220) F(240) AND 
CONT C(68) C(71) F(221) F(241) F(230) AND 
CONT C(68) C(71) F(241) F(230) F(221) AND 
CONT C(68) C(71) F(230) F(221) F(241) 
DELU 0.015 C(68) C(71) F(220) F(240) F(231) AND 
CONT C(68) C(71) F(240) F(231) F(220) AND 
CONT C(68) C(71) F(231) F(220) F(240) AND 
CONT C(68) C(71) F(221) F(241) F(230) AND 
CONT C(68) C(71) F(241) F(230) F(221) AND 
CONT C(68) C(71) F(230) F(221) F(241) 
SIMU 0.015 C(68) C(71) F(220) F(240) F(231) AND 
CONT C(68) C(71) F(240) F(231) F(220) AND 
CONT C(68) C(71) F(231) F(220) F(240) AND 
CONT C(68) C(71) F(221) F(241) F(230) AND 
CONT C(68) C(71) F(241) F(230) F(221) AND 
CONT C(68) C(71) F(230) F(221) F(241) 
DELU 0.015 C(250) C(270) C(260) AND 
CONT C(260) C(270) C(250) 
SIMU 0.015 C(250) C(270) C(260) AND 
CONT C(260) C(270) C(250) 
DELU 0.015 C(251) C(271) C(261) AND 
CONT C(261) C(271) C(251) 
SIMU 0.015 C(251) C(271) C(261) AND 
CONT C(261) C(271) C(251) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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