Ortho-aryl substituted DPEphos ligands: Rhodium Complexes Featuring C‒H Anagostic Interactions and B‒H Agostic Bonds.
Race, James; Burnage, Arron; Boyd, Timothy M.; Heyam, Alex; Martinez-Martinez, Antonio J.; Macgregor, Stuart Alan; Weller, Andrew S.; Chemical Science  (2021) –; doi:10.1039/D1SC01430G

data_1562853
_publ_section_title
;
 Ortho-aryl substituted DPEphos ligands: Rhodium Complexes Featuring C--H
 Anagostic Interactions and B--H Agostic Bonds.
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC01430G
_journal_year                    2021
_chemical_formula_moiety         'C47 H44 O P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C79 H56 B F24 O P2 Rh'
_chemical_formula_weight         1652.89
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-09-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-02-21 deposited with the CCDC.	2021-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                81.607(2)
_cell_angle_beta                 84.6750(10)
_cell_angle_gamma                84.5080(10)
_cell_formula_units_Z            2
_cell_length_a                   13.1702(2)
_cell_length_b                   15.7363(3)
_cell_length_c                   17.8817(3)
_cell_measurement_reflns_used    42365
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.5560
_cell_measurement_theta_min      2.5040
_cell_volume                     3637.75(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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    -98.00 -69.00   1.00    1.00    --    0.00-178.00  30.00   29
  2  \w    -89.00 -43.00   1.00    1.00    --    0.00 178.00  60.00   46
  3  \w    -61.00 -36.00   1.00    1.00    --    0.00-178.00  30.00   25
  4  \w    -37.00  42.00   1.00    1.00    --    0.00  57.00 -30.00   79
  5  \w     50.00  91.00   1.00    1.00    --    0.00  57.00 -30.00   41
  6  \w    -32.00  29.00   1.00    3.00    --  -60.50  30.00  90.00   61
  7  \w    -30.00  29.00   1.00    3.00    --  -60.50  30.00-120.00   59
  8  \w   -145.00 -79.00   1.00    3.00    --  -60.50-125.00-120.00   66
  9  \w   -122.00 -93.00   1.00    3.00    --  -60.50 -94.00 -30.00   29
 10  \w    -83.00 -34.00   1.00    3.00    --  -60.50 125.00  30.00   49
 11  \w     35.00 116.00   1.00    3.00    --   60.50-125.00   0.00   81
 12  \w    -14.00  91.00   1.00    3.00    --   60.50 -30.00-150.00  105
 13  \w    100.00 152.00   1.00    3.00    --   60.50 125.00-120.00   52
 14  \w     96.00 150.00   1.00    3.00    --   60.50 125.00 -60.00   54
 15  \w    -40.00   6.00   1.00    3.00    --   60.50 -77.00-180.00   46
 16  \w    103.00 128.00   1.00    3.00    --   60.50 125.00-180.00   25
 17  \w     41.00  95.00   1.00    3.00    --   60.50 -77.00-180.00   54
 18  \w     76.00 112.00   1.00    6.00    --  121.00-111.00 -60.00   36
 19  \w     32.00  78.00   1.00    6.00    --  121.00 -37.00 150.00   46
 20  \w     35.00  60.00   1.00    6.00    --  121.00-111.00 -60.00   25
 21  \w     77.00 112.00   1.00    6.00    --  121.00-111.00-180.00   35
 22  \w     61.00 111.00   1.00    6.00    --  121.00-111.00  60.00   50
 23  \w     51.00 104.00   1.00    6.00    --  121.00 -50.00 -90.00   53
 24  \w     78.00 146.00   1.00    6.00    --  121.00 178.00 -60.00   68
 25  \w     62.00  88.00   1.00    6.00    --  121.00-111.00 -30.00   26
 26  \w     41.00  80.00   1.00    6.00    --  121.00 -25.00 -30.00   39
 27  \w     43.00  84.00   1.00    6.00    --  121.00 -37.00 -60.00   41
 28  \w     82.00 108.00   1.00    6.00    --  121.00-111.00 120.00   26
 29  \w     73.00 111.00   1.00    6.00    --  121.00-111.00   0.00   38
 30  \w     30.00  67.00   1.00    6.00    --  121.00 -37.00  30.00   37
 31  \w     29.00 110.00   1.00    6.00    --  121.00-111.00 -90.00   81
 32  \w     34.00  60.00   1.00    6.00    --  121.00-111.00 120.00   26
 33  \w     86.00 112.00   1.00    6.00    --  121.00-111.00 150.00   26
 34  \w     62.00  89.00   1.00    6.00    --  121.00 -50.00 150.00   27
 35  \w     32.00  94.00   1.00    6.00    --  121.00 -25.00-120.00   62
 36  \w     64.00  89.00   1.00    6.00    --  121.00-111.00  30.00   25
 37  \w     41.00  99.00   1.00    6.00    --  121.00 -50.00-150.00   58
 38  \w     74.00 170.00   1.00    6.00    --  121.00  37.00 150.00   96
 39  \w     44.00  70.00   1.00    6.00    --  121.00 -50.00  90.00   26
 40  \w     24.00 173.00   1.00    6.00    --  121.00   0.00 -60.00  149
 41  \w     80.00 105.00   1.00    6.00    --  121.00 -50.00 -60.00   25
 42  \w    114.00 175.00   1.00    6.00    --  121.00 111.00 -60.00   61
 43  \w     50.00 149.00   1.00    6.00    --  121.00 -63.00  30.00   99
 44  \w    -46.00 -21.00   1.00    3.00    --  -60.50  57.00-142.00   25
 45  \w      6.00  33.00   1.00    1.00    --    0.00 -77.00-150.00   27
 46  \w    -23.00   5.00   1.00    1.00    --    0.00 -77.00-150.00   28
 47  \w   -100.00 -74.00   1.00    1.00    --    0.00 -77.00-150.00   26
 48  \w    -69.00 -29.00   1.00    1.00    --    0.00 -77.00-150.00   40
 49  \w    -99.00 -34.00   1.00    1.00    --    0.00 178.00-150.00   65
 50  \w    -26.00  -1.00   1.00    3.00    --   38.00 122.00 -17.30   25
 51  \w    -23.00   3.00   1.00    3.00    --   38.00 117.00 163.58   26
 52  \w      2.00  27.00   1.00    3.00    --   50.00  92.00  84.19   25
 53  \w      9.00  34.00   1.00    3.00    --   54.00  85.00 129.87   25
 54  \w      8.00  33.00   1.00    3.00    --   54.00  87.00 -25.74   25
 55  \w     16.00  41.00   1.00    3.00    --   60.50  82.00 161.01   25
 56  \w     16.00  41.00   1.00    3.00    --   60.50  81.00 -77.84   25
 57  \w     16.00  45.00   1.00    3.00    --   60.50  82.00  23.18   29
 58  \w     16.00  45.00   1.00    3.00    --   60.50  82.00  84.49   29
 59  \w     17.00  45.00   1.00    3.00    --   60.50  82.00-144.73   28
 60  \w     18.00  43.00   1.00    3.00    --   62.00  82.00-179.20   25
 61  \w     26.00 100.00   1.00    3.00    --   66.00  73.00 -48.10   74
 62  \w     70.00 130.00   1.00    3.00    --   66.00  73.00  -5.32   60
 63  \w     24.00  50.00   1.00    3.00    --   66.00  73.00  -5.32   26
 64  \w     27.00  60.00   1.00    3.00    --   70.00  70.00 135.53   33
 65  \w     75.00 138.00   1.00    3.00    --   70.00  70.00 135.53   63
 66  \w     32.00 119.00   1.00    3.00    --   74.00  72.00-124.73   87
 67  \w     35.00  84.00   1.00    3.00    --   78.00  66.00  99.96   49
 68  \w     41.00  67.00   1.00    3.00    --   82.00  67.00 -38.98   26
 69  \w     39.00  65.00   1.00    3.00    --   82.00  72.00  25.50   26
 70  \w     39.00  65.00   1.00    3.00    --   82.00  76.00 157.82   26
 71  \w     79.00 116.00   1.00    3.00    --   86.00  64.00 -81.04   37
 72  \w     41.00  73.00   1.00    3.00    --   86.00  64.00 -81.04   32
 73  \w     42.00  94.00   1.00    3.00    --   86.00  77.00  43.35   52
 74  \w     43.00  69.00   1.00    3.00    --   86.00  73.00 -11.26   26
 75  \w     45.00  92.00   1.00    3.00    --   90.00  64.00-172.62   47
 76  \w     48.00  97.00   1.00    3.00    --   90.00  72.00 117.39   49
 77  \w     55.00  96.00   1.00    6.00    --   98.00  70.00-170.45   41
 78  \w     58.00 104.00   1.00    6.00    --  102.00  77.00-159.99   46
 79  \w     63.00  90.00   1.00    6.00    --  106.00  75.00 -16.37   27
 80  \w     65.00 111.00   1.00    6.00    --  106.00  53.00  94.85   46
 81  \w     75.00 100.00   1.00    6.00    --  118.00  71.00 125.87   25
 82  \w    113.00 139.00   1.00    6.00    --  121.00  63.00  90.00   26
 83  \w     77.00 102.00   1.00    6.00    --  121.00  63.00  90.00   25
 84  \w     77.00 127.00   1.00    6.00    --  121.00  77.00-150.00   50
 85  \w     77.00 167.00   1.00    6.00    --  121.00  63.00 -30.00   90
 86  \w    140.00 166.00   1.00    6.00    --  121.00  77.00 -90.00   26
 87  \w     77.00 116.00   1.00    6.00    --  121.00  77.00 -90.00   39
 88  \w     77.00 127.00   1.00    6.00    --  121.00  77.00 150.00   50
 89  \w     77.00 149.00   1.00    6.00    --  121.00  77.00   0.00   72
 90  \w     77.00 164.00   1.00    6.00    --  121.00  63.00 -60.00   87
 91  \w     77.00 157.00   1.00    6.00    --  121.00  63.00  60.00   80
 92  \w     78.00 104.00   1.00    6.00    --  121.00  63.00 150.00   26
 93  \w     77.00 123.00   1.00    6.00    --  121.00  77.00-180.00   46
 94  \w     78.00 113.00   1.00    6.00    --  121.00  63.00-120.00   35
 95  \w     77.00 138.00   1.00    6.00    --  121.00  63.00  30.00   61
 96  \w     78.00 122.00   1.00    6.00    --  121.00  74.00-106.99   44
 97  \w     77.00 132.00   1.00    6.00    --  121.00  63.00   0.00   55
 98  \w     80.00 146.00   1.00    6.00    --  121.00  77.00  90.00   66
 99  \w    145.00 178.00   1.00    6.00    --  121.00  77.00-120.00   33
100  \w     77.00 155.00   1.00    6.00    --  121.00  77.00  30.00   78
101  \w     77.00 115.00   1.00    6.00    --  121.00  77.00-120.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            68981
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.684
_diffrn_reflns_theta_min         2.506
_exptl_absorpt_coefficient_mu    3.271
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       prism
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         15179
_refine_ls_number_restraints     690
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+3.7532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1146
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14437
_reflns_number_total             15179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01430g3.cif
_cod_data_source_block           2-Me
_cod_database_code               1562853
_publcif_datablock.id            {dca5f9aa-b3b0-4209-86a2-cdc29cbc6040}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.623
_shelx_estimated_absorpt_t_min   0.561
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F9-F8 \\sim F9-F7 \\sim F8-F7 \\sim F9A-F8A \\sim F9A-F7A \\sim F8A-F7A
 with sigma of 0.04
 C62-F9 \\sim C62-F8 \\sim C62-F7 \\sim C62-F9A \\sim C62-F8A \\sim C62-F7A
 with sigma of 0.02
 F5A-F6A \\sim F5A-F4A \\sim F5-F6 \\sim F5-F4 \\sim F6A-F4A \\sim F6-F4
 with sigma of 0.04
 C55-F5A \\sim C55-F5 \\sim C55-F6A \\sim C55-F6 \\sim C55-F4 \\sim C55-F4A
 with sigma of 0.02
 F16A-F18A \\sim F16A-F17A \\sim F16-F18 \\sim F16-F17 \\sim F18A-F17A \\sim
F18-F17
 with sigma of 0.04
 C71-F16A \\sim C71-F16 \\sim C71-F18A \\sim C71-F18 \\sim C71-F17A \\sim
C71-F17
 with sigma of 0.02
 F23-F24 \\sim F23-F22 \\sim F24-F22 \\sim F23A-F24A \\sim F23A-F22A \\sim
F24A-F22A
 with sigma of 0.04
 C79-F23 \\sim C79-F24 \\sim C79-F22 \\sim C79-F23A \\sim C79-F24A \\sim
C79-F22A
 with sigma of 0.02
 F13-F14 \\sim F13-F15 \\sim F13A-F14A \\sim F13A-F15A \\sim F14-F15 \\sim
F14A-F15A
 with sigma of 0.04
 C70-F13 \\sim C70-F13A \\sim C70-F14 \\sim C70-F14A \\sim C70-F15 \\sim
C70-F15A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C62 \\sim F7 \\sim F8 \\sim F9 \\sim F7A \\sim F8A \\sim F9A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C55 \\sim F4 \\sim F5 \\sim F6 \\sim F4A \\sim F5A \\sim F6A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C71 \\sim F16 \\sim F17 \\sim F18 \\sim F16A \\sim F17A \\sim F18A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C79 \\sim F22 \\sim F23 \\sim F24 \\sim F22A \\sim F23A \\sim F24A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C70 \\sim F13 \\sim F14 \\sim F15 \\sim F13A \\sim F14A \\sim F15A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
Uanis(F7) = Uanis(F7A)
Uanis(F7A) = Uanis(F7)
4. Rigid body (RIGU) restrains
 C62, F7, F8, F9, F7A, F8A, F9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C55, F4, F5, F6, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C71, F16, F17, F18, F16A, F17A, F18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C79, F22, F23, F24, F22A, F23A, F24A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C70, F13, F14, F15, F13A, F14A, F15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(3)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(3)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(4)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(4)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(5)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C40(H40), C41(H41), C42(H42), C37(H37), C38(H38), C39(H39)
6.b Secondary CH2 refined with riding coordinates:
 C43(H43a,H43b)
6.c Aromatic/amide H refined with riding coordinates:
 C49(H49), C51(H51), C53(H53), C57(H57), C59(H59), C61(H61), C65(H65),
 C67(H67), C69(H69), C73(H73), C75(H75), C77(H77), C17(H17), C16(H16), C15(H15),
  C14(H14), C20(H20), C21(H21), C22(H22), C23(H23), C4(H4), C3(H3), C2(H2),
 C1(H1), C11(H11), C10(H10), C9(H9), C8(H8), C29(H29), C28(H28), C27(H27),
 C26(H26), C35(H35), C34(H34), C33(H33), C32(H32)
6.d Idealised Me refined as rotating group:
 C44(H44a,H44b,H44c), C45(H45a,H45b,H45c), C46(H46a,H46b,H46c), C47(H47a,H47b,
 H47c)
;
_shelx_res_checksum              21905
_shelx_hkl_checksum              39167
_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
;
_publcif_funding_html
;
;