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_1562857
_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         'C51 H60 B N O P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C83 H72 B2 F24 N O P2 Rh'
_chemical_formula_weight         1741.88
_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   mixed
_audit_creation_date             2020-09-24
_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                114.334(3)
_cell_angle_beta                 98.207(3)
_cell_angle_gamma                103.273(3)
_cell_formula_units_Z            2
_cell_length_a                   14.2087(6)
_cell_length_b                   17.3935(5)
_cell_length_c                   18.5698(6)
_cell_measurement_reflns_used    9660
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      75.5660
_cell_measurement_theta_min      2.7010
_cell_volume                     3921.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_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    -39.00  11.00   1.00    1.00    --    0.00  57.00 -60.00   50
  2  \w     17.00  90.00   1.00    1.00    --    0.00  57.00 -60.00   73
  3  \w    -94.00 -62.00   1.00    1.00    --    0.00-178.00-150.00   32
  4  \w    -77.00 -37.00   1.00    1.00    --    0.00 178.00  30.00   40
  5  \w   -143.00-103.00   1.00   11.00    --  -60.50 -94.00 -60.00   40
  6  \w   -147.00-121.00   1.00   11.00    --  -60.50 -94.00 120.00   26
  7  \w   -145.00  38.00   1.00   11.00    --  -60.50 -15.00-180.00  183
  8  \w    102.00 152.00   1.00   11.00    --   60.50 125.00 120.00   50
  9  \w     26.00 117.00   1.00   11.00    --   60.50-125.00-150.00   91
 10  \w    107.00 151.00   1.00   11.00    --   60.50 125.00 -30.00   44
 11  \w     94.00 152.00   1.00   11.00    --   60.50 125.00-120.00   58
 12  \w     95.00 122.00   1.00   11.00    --   60.50 125.00 -90.00   27
 13  \w    112.00 144.00   1.00   11.00    --   60.50 125.00  60.00   32
 14  \w     95.00 120.00   1.00   11.00    --   60.50 125.00-180.00   25
 15  \w     24.00  79.00   1.00   11.00    --   60.50-125.00  90.00   55
 16  \w    127.00 152.00   1.00   11.00    --   60.50 125.00  30.00   25
 17  \w     51.00 110.00   1.00   20.00    --  121.00-111.00  30.00   59
 18  \w     64.00  92.00   1.00   20.00    --  121.00 -25.00  30.00   28
 19  \w     28.00  86.00   1.00   20.00    --  121.00 -25.00-150.00   58
 20  \w     34.00  60.00   1.00   20.00    --  121.00 -25.00  30.00   26
 21  \w     44.00  90.00   1.00   20.00    --  121.00-111.00-150.00   46
 22  \w     28.00  94.00   1.00   20.00    --  121.00 -25.00 -30.00   66
 23  \w     33.00  82.00   1.00   20.00    --  121.00 -50.00  60.00   49
 24  \w     24.00 176.00   1.00   20.00    --  121.00   0.00 150.00  152
 25  \w     45.00 112.00   1.00   20.00    --  121.00-111.00-180.00   67
 26  \w     46.00 104.00   1.00   20.00    --  121.00 -50.00-150.00   58
 27  \w     29.00  86.00   1.00   20.00    --  121.00 -25.00 150.00   57
 28  \w     76.00 112.00   1.00   20.00    --  121.00-111.00 -60.00   36
 29  \w     35.00  62.00   1.00   20.00    --  121.00 -25.00 -60.00   27
 30  \w    111.00 137.00   1.00   20.00    --  121.00 -77.00-150.00   26
 31  \w     59.00 150.00   1.00   20.00    --  121.00 178.00  90.00   91
 32  \w     85.00 110.00   1.00   20.00    --  121.00-111.00   0.00   25
 33  \w     33.00  94.00   1.00   20.00    --  121.00 -25.00  90.00   61
 34  \w     34.00 103.00   1.00   20.00    --  121.00 -50.00   0.00   69
 35  \w     86.00 112.00   1.00   20.00    --  121.00-111.00 150.00   26
 36  \w     71.00 111.00   1.00   20.00    --  121.00-111.00 120.00   40
 37  \w     82.00 108.00   1.00   20.00    --  121.00 -77.00   0.00   26
 38  \w    128.00 159.00   1.00   20.00    --  121.00 -77.00   0.00   31
 39  \w     73.00 112.00   1.00   20.00    --  121.00-111.00-120.00   39
 40  \w     64.00  92.00   1.00   20.00    --  121.00 -37.00-120.00   28
 41  \w     32.00  65.00   1.00   20.00    --  121.00 -25.00 -90.00   33
 42  \w     64.00 112.00   1.00   20.00    --  121.00-111.00  60.00   48
 43  \w     30.00  95.00   1.00   20.00    --  121.00 -77.00-150.00   65
 44  \w    -57.00 -31.00   1.00    1.00    --    0.00 -49.00-138.00   26
 45  \w     48.00  90.00   1.00    1.00    --    0.00  37.00-120.00   42
 46  \w      1.00  42.00   1.00    1.00    --    0.00 -99.00 120.00   41
 47  \w    -12.00  30.00   1.00    1.00    --    0.00 -49.00-138.00   42
 48  \w    -40.00  37.00   1.00    1.00    --    0.00  37.00-120.00   77
 49  \w    -34.00  -9.00   1.00   11.00    --   34.00 130.00-115.53   25
 50  \w    -29.00  -4.00   1.00   11.00    --   34.00 121.00  54.49   25
 51  \w      2.00  27.00   1.00   11.00    --   50.00  92.00  62.28   25
 52  \w      9.00  34.00   1.00   11.00    --   54.00  86.00 -69.91   25
 53  \w      8.00  33.00   1.00   11.00    --   54.00  87.00-168.50   25
 54  \w     10.00  35.00   1.00   11.00    --   54.00  84.00   7.49   25
 55  \w     21.00  46.00   1.00   11.00    --   60.50  77.00 -60.00   25
;
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37813
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.828
_diffrn_reflns_theta_min         2.710
_exptl_absorpt_coefficient_mu    3.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
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    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1087
_refine_ls_number_reflns         16262
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0787P)^2^+1.2006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12096
_reflns_number_total             16262
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01430g3.cif
_cod_data_source_block           6-iPr
_cod_database_code               1562857
_publcif_datablock.id            {165c8ff9-98c2-4c9c-bd88-f5ded34234f0}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.862
_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. Restrained distances
 F1-F2 \\sim F1-F3 \\sim F2-F3 \\sim F2A-F1A \\sim F2A-F3A \\sim F1A-F3A
 with sigma of 0.04
 C66-C65 \\sim C66-F1 \\sim C66-F2 \\sim C66-F3 \\sim C66-F2A \\sim C66-F1A
\\sim C66-F3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Rh1A) \\sim Ueq, Uanis(Rh1) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 F2A, F1A, F3A, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F3, F2, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F2A)=Sof(F1A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(Rh1A)=1-FVAR(2)
 Sof(Rh1)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C46(H46), C43(H43), C49(H49)
6.b Aromatic/amide H refined with riding coordinates:
 C77(H77), C53(H53), C83(H83), C26(H26), C69(H69), C9(H9), C67(H67), C56(H56),
 C75(H75), C64(H64), C61(H61), C17(H17), C8(H8), C27(H27), C80(H80), C20(H20),
 C35(H35), C14(H14), C10(H10), C22(H22), C59(H59), C34(H34), C23(H23), C16(H16),
  C1(H1), C15(H15), C72(H72), C11(H11), C32(H32), C21(H21), C33(H33), C28(H28),
 C29(H29), C2(H2), C3(H3), C4(H4)
6.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C47(H47A,H47B,
 H47C), C42(H42A,H42B,H42C), C51(H51A,H51B,H51C), C44(H44A,H44B,H44C), C41(H41A,
 H41B,H41C), C50(H50A,H50B,H50C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              3174
_shelx_hkl_checksum              99345
_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
;
;