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_1562854
_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         'C55 H60 O P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C87 H72 B F24 O P2 Rh'
_chemical_formula_weight         1765.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 113.5620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.43890(10)
_cell_length_b                   18.04470(10)
_cell_length_c                   24.4986(2)
_cell_measurement_reflns_used    61283
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      76.1560
_cell_measurement_theta_min      3.6610
_cell_volume                     8282.12(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -44.00  23.00   1.00    2.40    --  -42.66  38.00 -60.00   67
  2  \w   -109.00 -21.00   1.00    2.40    --  -42.66 -38.00 150.00   88
  3  \w     14.00  65.00   1.00    2.40    --   42.66 -38.00  30.00   51
  4  \w    -30.00   6.00   1.00    2.40    --   42.66 -38.00  30.00   36
  5  \w     92.00 171.00   1.00    9.57    --  111.00  45.00 -90.00   79
  6  \w     48.00 100.00   1.00    9.57    --  111.00 -95.00 120.00   52
  7  \w     45.00  86.00   1.00    9.57    --  111.00 -30.00 -60.00   41
  8  \w     47.00 132.00   1.00    9.57    --  111.00 -61.00 -30.00   85
  9  \w    111.00 138.00   1.00    9.57    --  111.00  15.00-150.00   27
 10  \w     61.00 115.00   1.00    9.57    --  111.00-125.00 -60.00   54
 11  \w     33.00  74.00   1.00    9.57    --  111.00 -95.00 150.00   41
 12  \w     58.00  88.00   1.00    9.57    --  111.00 -30.00-150.00   30
 13  \w     75.00 112.00   1.00    9.57    --  111.00-125.00-120.00   37
 14  \w     82.00 107.00   1.00    9.57    --  111.00  15.00-150.00   25
 15  \w     42.00  79.00   1.00    9.57    --  111.00 -45.00 150.00   37
 16  \w    142.00 168.00   1.00    9.57    --  111.00  15.00-150.00   26
 17  \w     45.00  82.00   1.00    9.57    --  111.00 -45.00-180.00   37
 18  \w     91.00 131.00   1.00    9.57    --  111.00  61.00  90.00   40
 19  \w     93.00 175.00   1.00    9.57    --  111.00  30.00-120.00   82
 20  \w     -5.00  29.00   1.00    2.40    --  -42.66  38.00 -30.00   34
 21  \w     59.00 125.00   1.00    2.40    --   42.66 178.00  90.00   66
 22  \w     15.00  41.00   1.00    2.40    --   42.66 -38.00   0.00   26
 23  \w    -29.00  -4.00   1.00    2.40    --   42.66 -38.00   0.00   25
 24  \w     90.00 129.00   1.00    2.40    --   42.66 178.00 -90.00   39
 25  \w     92.00 118.00   1.00    9.57    --  111.00-125.00   0.00   26
 26  \w     41.00  75.00   1.00    9.57    --  111.00-125.00   0.00   34
 27  \w     55.00  82.00   1.00    9.57    --  111.00 -45.00 -90.00   27
 28  \w     43.00  95.00   1.00    9.57    --  111.00-125.00 120.00   52
 29  \w     57.00  83.00   1.00    9.57    --  111.00-125.00 150.00   26
 30  \w     52.00  87.00   1.00    9.57    --  111.00 -77.00-150.00   35
 31  \w     91.00 140.00   1.00    9.57    --  111.00 -77.00-150.00   49
 32  \w     93.00 118.00   1.00    9.57    --  111.00-125.00-120.00   25
 33  \w    116.00 142.00   1.00    9.57    --  111.00 -77.00 -60.00   26
 34  \w    129.00 155.00   1.00    9.57    --  111.00 125.00 -60.00   26
 35  \w     70.00  96.00   1.00    9.57    --  111.00 -45.00  90.00   26
 36  \w     42.00  68.00   1.00    9.57    --  111.00 -45.00  90.00   26
 37  \w     86.00 112.00   1.00    9.57    --  111.00-125.00  90.00   26
 38  \w     85.00 125.00   1.00    9.57    --  111.00  15.00  60.00   40
 39  \w     93.00 118.00   1.00    9.57    --  111.00-125.00 150.00   25
 40  \w     83.00 115.00   1.00    9.57    --  111.00-125.00-150.00   32
 41  \w     95.00 121.00   1.00    9.57    --  111.00 125.00   0.00   26
 42  \w    153.00 178.00   1.00    9.57    --  111.00 125.00   0.00   25
 43  \w    128.00 156.00   1.00    9.57    --  111.00 125.00  60.00   28
 44  \w     40.00  99.00   1.00    9.57    --  111.00-125.00  30.00   59
 45  \w    107.00 177.00   1.00    9.57    --  111.00  15.00 -30.00   70
 46  \w     39.00  70.00   1.00    9.57    --  111.00-125.00  90.00   31
 47  \w     86.00 118.00   1.00    9.57    --  111.00-125.00  60.00   32
 48  \w     40.00  85.00   1.00    9.57    --  111.00 -30.00  90.00   45
 49  \w      2.00  27.00   1.00    2.40    --   38.00  90.00-160.20   25
 50  \w    -52.00 -25.00   1.00    2.40    --  -42.66 -38.00  60.00   27
 51  \w    -73.00 -14.00   1.00    2.40    --  -42.66 -19.00-180.00   59
 52  \w    -53.00 -16.00   1.00    2.40    --  -42.66 -57.00  30.00   37
 53  \w   -109.00 -16.00   1.00    2.40    --  -42.66 -57.00 -60.00   93
 54  \w   -112.00 -57.00   1.00    2.40    --  -42.66 -57.00  30.00   55
 55  \w     79.00 126.00   1.00    2.40    --   42.66-178.00   0.00   47
 56  \w     17.00  42.00   1.00    2.40    --   50.00  82.00  48.16   25
 57  \w     18.00  43.00   1.00    2.40    --   50.00  81.00 163.08   25
 58  \w     18.00  43.00   1.00    2.40    --   50.00  81.00-144.11   25
 59  \w     17.00  42.00   1.00    2.40    --   50.00  82.00 -78.23   25
 60  \w     18.00  43.00   1.00    2.40    --   50.00  81.00 -11.51   25
 61  \w     19.00  45.00   1.00    2.40    --   50.00  81.00 105.40   26
 62  \w     33.00  59.00   1.00    2.40    --   62.00  77.00 121.74   26
 63  \w     32.00  57.00   1.00    2.40    --   62.00  76.00-113.14   25
 64  \w     39.00  65.00   1.00    2.40    --   70.00  75.00 155.57   26
 65  \w     39.00  65.00   1.00    2.40    --   70.00  76.00-169.45   26
 66  \w     39.00  65.00   1.00    2.40    --   70.00  76.00  54.97   26
 67  \w     40.00  65.00   1.00    2.40    --   70.00  76.00 -98.27   25
 68  \w     43.00  69.00   1.00    2.40    --   74.00  77.00  70.74   26
 69  \w     43.00  69.00   1.00    2.40    --   74.00  77.00 113.15   26
 70  \w     43.00  69.00   1.00    2.40    --   74.00  77.00 -11.14   26
 71  \w     43.00  69.00   1.00    2.40    --   74.00  77.00  12.27   26
 72  \w    107.00 148.00   1.00    2.40    --   74.00  77.00 -67.80   41
 73  \w     43.00  69.00   1.00    2.40    --   74.00  75.00 -29.26   26
 74  \w     43.00  68.00   1.00    2.40    --   74.00  75.00-141.51   25
 75  \w     43.00  69.00   1.00    2.40    --   74.00  77.00 -67.80   26
 76  \w     43.00  68.00   1.00    2.40    --   74.00  77.00 -86.15   25
 77  \w     48.00  74.00   1.00    9.57    --   78.00  70.00  -3.37   26
 78  \w     55.00  81.00   1.00    9.57    --   82.00  60.00  98.33   26
 79  \w     57.00  82.00   1.00    9.57    --   86.00  66.00-166.01   25
 80  \w     61.00  87.00   1.00    9.57    --   86.00  56.00  43.13   26
 81  \w     58.00  84.00   1.00    9.57    --   86.00  76.00-123.47   26
 82  \w     63.00  88.00   1.00    9.57    --   90.00  59.00 173.68   25
 83  \w     61.00  91.00   1.00    9.57    --   90.00  70.00 117.47   30
 84  \w    132.00 161.00   1.00    9.57    --   90.00  70.00 -47.54   29
 85  \w     61.00  68.00   1.00    9.57    --   90.00  70.00 -47.54    7
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0505504000
_diffrn_orient_matrix_UB_12      0.0673351000
_diffrn_orient_matrix_UB_13      0.0173421000
_diffrn_orient_matrix_UB_21      -0.0419683000
_diffrn_orient_matrix_UB_22      0.0345631000
_diffrn_orient_matrix_UB_23      -0.0616945000
_diffrn_orient_matrix_UB_31      -0.0494705000
_diffrn_orient_matrix_UB_32      0.0395088000
_diffrn_orient_matrix_UB_33      0.0244627000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            155774
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.221
_diffrn_reflns_theta_min         3.401
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.909
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             3592
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1175
_refine_ls_number_reflns         17246
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+4.5858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14838
_reflns_number_total             17246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01430g3.cif
_cod_data_source_block           2-iPr
_cod_database_code               1562854
_publcif_datablock.id            {7b83adcf-e1d6-4ea1-a79c-5698894d1eb6}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C60 H60 Rh1 P2 O1 B1 F24'
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.594
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
 F9A-F7A \\sim F7A-F8A
 with sigma of 0.02
 F9-F7 \\sim F7-F8
 with sigma of 0.02
 F4A-F5A \\sim F5A-F6A
 with sigma of 0.02
 F4-F5 \\sim F5-F6
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C67, F5A, F6A, F4A, F4, F5, F6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F12, F11, F10, C75, F12A, F10A, F11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F9, F7, F8, C86, F9A, F8A, F7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F3, F2, F1, F3A, F1A, F2A, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F3A)=Sof(F1A)=Sof(F2A)=1-FVAR(1)
 Sof(F3)=Sof(F2)=Sof(F1)=FVAR(1)
 Sof(O1A)=1-FVAR(2)
 Sof(O1)=FVAR(2)
 Sof(F9A)=Sof(F8A)=Sof(F7A)=1-FVAR(3)
 Sof(F9)=Sof(F7)=Sof(F8)=FVAR(3)
 Sof(F12A)=Sof(F10A)=Sof(F11A)=1-FVAR(4)
 Sof(F12)=Sof(F11)=Sof(F10)=FVAR(4)
 Sof(F4)=Sof(F5)=Sof(F6)=1-FVAR(5)
 Sof(F5A)=Sof(F6A)=Sof(F4A)=FVAR(5)
5.a Ternary CH refined with riding coordinates:
 C37(H37), C38(H38), C42(H42), C39(H39), C50(H50), C41(H41), C40(H40),
 C53(H53), C47(H47), C44(H44)
5.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B)
5.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C8(H8), C57(H57), C29(H29), C73(H73), C9(H9), C79(H79), C76(H76),
 C71(H71), C23(H23), C10(H10), C28(H28), C81(H81), C1(H1), C60(H60), C87(H87),
 C34(H34), C11(H11), C35(H35), C63(H63), C27(H27), C22(H22), C2(H2), C68(H68),
 C32(H32), C84(H84), C33(H33), C65(H65), C14(H14), C17(H17), C16(H16), C20(H20),
  C3(H3), C4(H4), C21(H21), C15(H15)
5.d Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C46(H46A,H46B,H46C), C52(H52A,H52B,
 H52C), C48(H48A,H48B,H48C), C55(H55A,H55B,H55C), C54(H54A,H54B,H54C), C45(H45A,
 H45B,H45C)
;
_shelx_res_checksum              58961
_shelx_hkl_checksum              55372
_shelx_fab_checksum              92707
_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 1.213
_oxdiff_exptl_absorpt_empirical_full_min 0.900
_publcif_funding_html
;
;