Reversible dehydrogenation of a primary aryl borane.
MacNeil, Connor S.; Hsiang, Shou-Jen; Hayes, Paul G.; Chemical communications (Cambridge, England) 56 (2020) 12323–12326; doi:10.1039/d0cc05503d

data_7127200
_publ_section_title
;
 Reversible dehydrogenation of a primary aryl borane.
;
_journal_issue                   82
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12323
_journal_page_last               12326
_journal_paper_doi               10.1039/d0cc05503d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C43 H57 B F6 N3 O P2 Rh, C6 H6'
_chemical_formula_sum            'C49 H63 B F6 N3 O P2 Rh'
_chemical_formula_weight         999.68
_chemical_name_systematic        1-BArF
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-20 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.394(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.3648(5)
_cell_length_b                   12.21300(10)
_cell_length_c                   32.5843(5)
_cell_measurement_reflns_used    100312
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      27.4870
_cell_measurement_theta_min      2.5710
_cell_volume                     10510.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      7.00  53.00   0.50    7.12    --    2.54-126.00 126.00   92
  2  \w     15.00  64.00   0.50    7.12    --    2.54-144.00 -41.00   98
  3  \w      1.00  67.00   0.50    7.12    --    2.54  38.00 -60.00  132
  4  \w    -59.00  13.00   0.50    7.12    --    2.54 -57.00 120.00  144
  5  \w    -65.00   4.00   0.50    7.12    --    2.54 -19.00   0.00  138
  6  \w     -8.00  64.00   0.50    7.12    --    2.54  57.00 120.00  144
  7  \w    -59.00  13.00   0.50    7.12    --    2.54 -57.00  60.00  144
  8  \w      1.00  70.00   0.50    7.12    --    2.54  19.00-150.00  138
  9  \w     -8.00  64.00   0.50    7.12    --    2.54  57.00  60.00  144
 10  \w    -65.00   4.00   0.50    7.12    --    2.54 -19.00-120.00  138
 11  \w    -30.00  33.00   0.50    7.12    --    4.00 -89.00 -30.91  126
 12  \w    -42.00  17.00   0.50    7.12    --   -5.35 -77.00  90.00  118
 13  \w    -57.00 -29.00   0.50    7.12    --   -5.35 127.00-148.66   56
 14  \w    -59.00 -30.00   0.50    7.12    --   -5.35 130.00  70.49   58
 15  \w    -42.00  17.00   0.50    7.12    --   -5.35 -77.00 -90.00  118
 16  \w    -60.00 -30.00   0.50    7.12    --   -5.35 132.00  -1.36   60
 17  \w    -59.00 -30.00   0.50    7.12    --   -5.35 130.00 -58.01   58
 18  \w    -57.00 -29.00   0.50    7.12    --   -5.35 127.00  97.71   56
 19  \w    -42.00  17.00   0.50    7.12    --   -5.35 -77.00-150.00  118
 20  \w    -57.00 -29.00   0.50    7.12    --   -5.35 127.00 144.83   56
 21  \w    -59.00 -30.00   0.50    7.12    --   -5.35 130.00 -91.70   58
 22  \w    -59.00 -30.00   0.50    7.12    --   -5.35 130.00  27.57   58
 23  \w    -57.00 -29.00   0.50    7.12    --   -5.35 127.00-179.01   56
 24  \w     -2.00  49.00   0.50    7.12    --    4.00-116.00-139.63  102
 25  \w     -2.00  49.00   0.50    7.12    --    4.00-116.00 127.88  102
 26  \w    -55.00 -26.00   0.50    7.12    --   -5.35 124.00  56.28   58
 27  \w    -54.00 -26.00   0.50    7.12    --   -5.35 123.00 133.07   56
 28  \w    -58.00 -30.00   0.50    7.12    --   -5.35 129.00 -20.31   56
 29  \w    -42.00 -11.00   0.50    7.12    --   -5.35 -77.00-180.00   62
 30  \w    -59.00 -30.00   0.50    7.12    --   -5.35 130.00-117.80   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0220353000
_diffrn_orient_matrix_UB_12      0.0039536000
_diffrn_orient_matrix_UB_13      -0.0053700000
_diffrn_orient_matrix_UB_21      0.0152731000
_diffrn_orient_matrix_UB_22      0.0008235000
_diffrn_orient_matrix_UB_23      0.0227571000
_diffrn_orient_matrix_UB_31      0.0017360000
_diffrn_orient_matrix_UB_32      -0.0579085000
_diffrn_orient_matrix_UB_33      -0.0000382000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            235608
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.197
_diffrn_reflns_theta_min         2.386
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             4160
_exptl_crystal_preparation       'see SI'
_exptl_crystal_recrystallization_method 'see SI'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         11658
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+18.6213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10810
_reflns_number_total             11658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05503d2.cif
_cod_data_source_block           ph20001b
_cod_depositor_comments
'Adding full bibliography for 7127200--7127201.cif.'
_cod_database_code               7127200
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C43H55B1F6N3O1P2Rh1
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.777
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00N(H00N), C00O(H00O), C00R(H00R), C012(H012), C01B(H01S), C01J(H0AA)
2.b Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00F(H00F), C00H(H00H), C00K(H00K), C00P(H00P), C00Q(H00Q),
 C00S(H00S), C00W(H00W), C00Z(H00Z), C016(H016), C018(H018), C01C(H01T),
 C01H(H01Z), C01L(H3AA), C01M(H4AA), C01N(H5AA), C01Q(H6AA), C01R(H7AA),
 C01S(H8AA)
2.c Idealised Me refined as rotating group:
 C00V(H00A,H00B,H00C), C00X(H00D,H00G,H00I), C011(H01A,H01B,H01C), C013(H01D,
 H01E,H01F), C014(H01G,H01H,H01I), C015(H01J,H01K,H01L), C017(H01M,H01N,H01O),
 C01A(H01P,H01Q,H01R), C01F(H01W,H01X,H01Y), C01I(H01,H,HA), C01K(H1AA,HB,HC),
 C01O(H2AA,HD,HE)
;
_olex2_exptl_crystal_mounting_method 'MiTiGen loop paratone oil'
_olex2_submission_original_sample_id PH20001b
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.181
_oxdiff_exptl_absorpt_empirical_full_min 0.802