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_1562851
_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         'C48 H52 O P2'
_chemical_formula_sum            'C48 H52 O P2'
_chemical_formula_weight         706.83
_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                105.445(5)
_cell_angle_beta                 99.637(4)
_cell_angle_gamma                99.462(5)
_cell_formula_units_Z            2
_cell_length_a                   8.3692(5)
_cell_length_b                   13.6847(9)
_cell_length_c                   18.8298(8)
_cell_measurement_reflns_used    2069
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      60.5420
_cell_measurement_theta_min      4.8240
_cell_volume                     1999.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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      110.00(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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    -16.00  64.00   1.00    5.00    --   33.92 -77.00-120.00   80
  2  \w     -5.00  54.00   1.00    5.00    --   33.92 -57.00  90.00   59
  3  \w     20.00  81.00   1.00    5.00    --   33.92  57.00  90.00   61
  4  \w    -31.00  -4.00   1.00    5.00    --   33.92 -57.00 -30.00   27
  5  \w     14.00  99.00   1.00    5.00    --   33.92  57.00  30.00   85
  6  \w     21.00  81.00   1.00    5.00    --   33.92  37.00-120.00   60
  7  \w     52.00  88.00   1.00    5.00    --   33.92  57.00 -60.00   36
  8  \w    118.00 144.00   1.00   25.00    --   87.85 111.00-180.00   26
  9  \w     46.00 111.00   1.00   25.00    --   87.85 -45.00  90.00   65
 10  \w     24.00 105.00   1.00   25.00    --   87.85 -77.00-150.00   81
 11  \w     19.00  45.00   1.00   25.00    --   87.85 -45.00  90.00   26
 12  \w     58.00  96.00   1.00   25.00    --   87.85-111.00   0.00   38
 13  \w    108.00 144.00   1.00   25.00    --   87.85 178.00 -60.00   36
 14  \w    103.00 152.00   1.00   25.00    --   87.85  77.00-180.00   49
 15  \w     73.00 109.00   1.00   25.00    --   87.85  61.00-120.00   36
 16  \w     18.00 104.00   1.00   25.00    --   87.85 -45.00-120.00   86
 17  \w     20.00  98.00   1.00   25.00    --   87.85 -61.00  60.00   78
 18  \w     81.00 106.00   1.00   25.00    --   87.85-111.00-120.00   25
 19  \w     16.00 106.00   1.00   25.00    --   87.85 -94.00  30.00   90
 20  \w    121.00 147.00   1.00   25.00    --   87.85  77.00-120.00   26
 21  \w     15.00 161.00   1.00   25.00    --   87.85   0.00-180.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11012
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        61.202
_diffrn_reflns_theta_max         61.202
_diffrn_reflns_theta_min         4.821
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       needle
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         6053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0633P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4278
_reflns_number_total             6053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01430g3.cif
_cod_data_source_block           1-iPr
_cod_database_code               1562851
_publcif_datablock.id            {d5a2c1de-7e0f-49c0-8c38-2cae73463b16}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.789
_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:
 C37(H37), C43(H43), C46(H46), C40(H40)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C21(H21), C23(H23), C14(H14), C20(H20), C8(H8), C22(H22), C16(H16),
 C15(H15), C1(H1), C26(H26), C27(H27), C4(H4), C2(H2), C11(H11), C9(H9),
 C29(H29), C3(H3), C10(H10), C32(H32), C28(H28), C35(H35), C33(H33), C34(H34)
2.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C39(H39A,H39B,H39C), C38(H38A,H38B,
 H38C), C47(H47A,H47B,H47C), C41(H41A,H41B,H41C), C45(H45A,H45B,H45C), C42(H42A,
 H42B,H42C)
;
_shelx_res_checksum              24109
_shelx_hkl_checksum              7341
_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
;
;