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_1562855
_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         'C49 H52 O2 P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C81 H64 B F24 O2 P2 Rh'
_chemical_formula_weight         1700.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 110.1080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5769(2)
_cell_length_b                   16.50650(10)
_cell_length_c                   24.0640(2)
_cell_measurement_reflns_used    33538
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      76.0930
_cell_measurement_theta_min      3.4860
_cell_volume                     7675.20(12)
_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 (Sheldrick, 2015)'
_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    -41.00  -6.00   1.00    8.01    --  -42.66  38.00-120.00   35
  2  \w   -128.00 -34.00   1.00    8.01    --  -42.66 178.00   0.00   94
  3  \w   -113.00 -21.00   1.00    8.01    --  -42.66 -38.00 -90.00   92
  4  \w     58.00 139.00   1.00   32.04    --  111.00 -61.00 -60.00   81
  5  \w    141.00 167.00   1.00   32.04    --  111.00  30.00-180.00   26
  6  \w     57.00  88.00   1.00   32.04    --  111.00 -30.00   0.00   31
  7  \w     95.00 130.00   1.00   32.04    --  111.00  30.00-180.00   35
  8  \w     65.00 107.00   1.00   32.04    --  111.00 -95.00 -90.00   42
  9  \w     88.00 177.00   1.00   32.04    --  111.00  45.00  30.00   89
 10  \w     38.00  64.00   1.00   32.04    --  111.00 -30.00 -90.00   26
 11  \w     89.00 176.00   1.00   32.04    --  111.00  30.00 150.00   87
 12  \w    140.00 173.00   1.00   32.04    --  111.00 125.00 150.00   33
 13  \w     32.00  62.00   1.00   32.04    --  111.00 -95.00 -90.00   30
 14  \w     39.00  95.00   1.00   32.04    --  111.00-125.00 -30.00   56
 15  \w    115.00 140.00   1.00   32.04    --  111.00  89.00  47.00   25
 16  \w     41.00  71.00   1.00   32.04    --  111.00-125.00  30.00   30
 17  \w     91.00 117.00   1.00   32.04    --  111.00-125.00  30.00   26
 18  \w    125.00 162.00   1.00   32.04    --  111.00 125.00-150.00   37
 19  \w     48.00  90.00   1.00   32.04    --  111.00 -45.00  90.00   42
 20  \w    132.00 165.00   1.00   32.04    --  111.00 125.00   0.00   33
 21  \w   -107.00 -21.00   1.00    8.01    --  -42.66 -38.00   0.00   86
 22  \w    -19.00  16.00   1.00    8.01    --  -42.66  38.00-180.00   35
 23  \w     64.00 124.00   1.00    8.01    --   42.66 178.00   0.00   60
 24  \w     17.00  43.00   1.00    8.01    --   42.66  77.00  30.00   26
 25  \w     91.00 116.00   1.00    8.01    --   42.66  77.00  30.00   25
 26  \w     42.00 118.00   1.00   32.04    --  111.00-125.00-120.00   76
 27  \w     93.00 118.00   1.00   32.04    --  111.00-125.00 -30.00   25
 28  \w     73.00 118.00   1.00   32.04    --  111.00-125.00-180.00   45
 29  \w    125.00 171.00   1.00   32.04    --  111.00  45.00-150.00   46
 30  \w     45.00  73.00   1.00   32.04    --  111.00 -45.00  60.00   28
 31  \w     71.00 116.00   1.00   32.04    --  111.00-125.00 120.00   45
 32  \w     52.00  91.00   1.00   32.04    --  111.00 -30.00 120.00   39
 33  \w     68.00  98.00   1.00   32.04    --  111.00 -45.00-120.00   30
 34  \w     47.00  73.00   1.00   32.04    --  111.00-125.00  90.00   26
 35  \w     45.00  71.00   1.00   32.04    --  111.00-125.00 -60.00   26
 36  \w     87.00 113.00   1.00   32.04    --  111.00-125.00  90.00   26
 37  \w    107.00 136.00   1.00   32.04    --  111.00 -61.00  60.00   29
 38  \w     40.00  66.00   1.00   32.04    --  111.00 -77.00 -90.00   26
 39  \w     76.00 102.00   1.00   32.04    --  111.00 -77.00 -90.00   26
 40  \w     85.00 111.00   1.00   32.04    --  111.00  15.00   0.00   26
 41  \w    130.00 156.00   1.00   32.04    --  111.00  15.00   0.00   26
 42  \w     42.00 112.00   1.00   32.04    --  111.00-125.00 -90.00   70
 43  \w    120.00 174.00   1.00   32.04    --  111.00  45.00  90.00   54
 44  \w     65.00 109.00   1.00   32.04    --  111.00 -77.00  90.00   44
 45  \w    102.00 128.00   1.00   32.04    --  111.00-138.00  67.87   26
;
_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      -0.0135497000
_diffrn_orient_matrix_UB_12      0.0832031000
_diffrn_orient_matrix_UB_13      0.0229428000
_diffrn_orient_matrix_UB_21      -0.0785499000
_diffrn_orient_matrix_UB_22      -0.0156126000
_diffrn_orient_matrix_UB_23      -0.0258522000
_diffrn_orient_matrix_UB_31      0.0025810000
_diffrn_orient_matrix_UB_32      -0.0392841000
_diffrn_orient_matrix_UB_33      0.0587576000
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            93147
_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         3.483
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89222
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             3448
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1036
_refine_ls_number_reflns         15989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+5.7282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13776
_reflns_number_total             15989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01430g3.cif
_cod_data_source_block           5-iPr
_cod_database_code               1562855
_publcif_datablock.id            {1b87c513-d086-4df6-86e6-fb9a08e71f76}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Rh1 P2 O1 N1 C30 H30'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Others
 Sof(F2A)=Sof(F3A)=Sof(F1A)=1-FVAR(1)
 Sof(F1)=Sof(F3)=Sof(F2)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C41(H41), C44(H44), C38(H38), C47(H47)
3.b Aromatic/amide H refined with riding coordinates:
 C67(H67), C73(H73), C51(H51), C59(H59), C75(H75), C78(H78), C57(H57),
 C81(H81), C17(H17), C54(H54), C1(H1), C4(H4), C2(H2), C23(H23), C70(H70),
 C3(H3), C8(H8), C16(H16), C21(H21), C62(H62), C26(H26), C29(H29), C65(H65),
 C15(H15), C14(H14), C9(H9), C11(H11), C20(H20), C28(H28), C22(H22), C10(H10),
 C27(H27), C32(H32), C34(H34), C33(H33), C35(H35)
3.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C49(H49A,H49B,H49C), C48(H48A,H48B,
 H48C), C46(H46A,H46B,H46C), C39(H39A,H39B,H39C), C43(H43A,H43B,H43C), C45(H45A,
 H45B,H45C)
;
_shelx_res_checksum              12448
_shelx_hkl_checksum              55453
_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 1.296
_oxdiff_exptl_absorpt_empirical_full_min 0.836
_publcif_funding_html
;
;