A family of rhodium(i) NHC chelates featuring O-containing tethers for catalytic tandem alkene isomerization-hydrosilylation.
Srivastava, Ravi; Jakoobi, Martin; Thieuleux, Chloé; Quadrelli, Elsje Alessandra; Camp, Clément; Dalton transactions (Cambridge, England : 2003) 50 (2021) 869–879; doi:10.1039/d0dt03698f

data_7705753
_publ_section_title
;
 A family of rhodium(i) NHC chelates featuring O-containing tethers for
 catalytic tandem alkene isomerization-hydrosilylation.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              869
_journal_page_last               879
_journal_paper_doi               10.1039/d0dt03698f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C24 H33 B F3 N2 O Rh'
_chemical_formula_sum            'C24 H33 B F3 N2 O Rh'
_chemical_formula_weight         536.24
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-31 deposited with the CCDC.	2020-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                65.159(7)
_cell_angle_beta                 82.202(6)
_cell_angle_gamma                83.726(7)
_cell_formula_units_Z            2
_cell_length_a                   7.6521(6)
_cell_length_b                   12.0807(9)
_cell_length_c                   14.3701(10)
_cell_measurement_reflns_used    16222
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.1690
_cell_measurement_theta_min      3.4600
_cell_volume                     1192.33(17)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.911
_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  63.00   1.00   15.71    --  -10.56  57.00-150.00  102
  2  \w    -84.00  18.00   1.00   15.71    --  -10.56 -57.00  60.00  102
  3  \w     -4.00  52.00   1.00   15.71    --   11.34 -99.00  90.00   56
  4  \w    -69.00  52.00   1.00   15.71    --   11.34 -19.00 150.00  121
  5  \w    -21.00  87.00   1.00   15.71    --   11.34  77.00 -30.00  108
  6  \w    -85.00  14.00   1.00   15.71    --  -10.56 -37.00 150.00   99
  7  \w    -81.00 -11.00   1.00   15.71    --  -10.56 147.00-134.23   70
  8  \w    -39.00  63.00   1.00   15.71    --  -10.56  57.00 120.00  102
  9  \w    -81.00 -11.00   1.00   15.71    --  -10.56 147.00 132.44   70
 10  \w     -4.00  52.00   1.00   15.71    --   11.34 -99.00   0.00   56
 11  \w    -86.00 -15.00   1.00   15.71    --  -10.56 154.00 -32.31   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0697735000
_diffrn_orient_matrix_UB_12      -0.0028080000
_diffrn_orient_matrix_UB_13      -0.0266416000
_diffrn_orient_matrix_UB_21      -0.0225647000
_diffrn_orient_matrix_UB_22      -0.0566700000
_diffrn_orient_matrix_UB_23      0.0407542000
_diffrn_orient_matrix_UB_31      -0.0583700000
_diffrn_orient_matrix_UB_32      0.0313080000
_diffrn_orient_matrix_UB_33      0.0248333000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31111
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.704
_diffrn_reflns_theta_min         2.918
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.095
_refine_diff_density_max         1.718
_refine_diff_density_min         -1.833
_refine_diff_density_rms         0.201
_refine_ls_extinction_coef       0.0139(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         6159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+8.9033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4902
_reflns_number_total             6159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03698f2.cif
_cod_data_source_block           rs181
_cod_depositor_comments
'Adding full bibliography for 7705753--7705755.cif.'
_cod_database_code               7705753
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H33 B1 F3 N2 O1 Rh1'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C18(H18), C22(H22), C21(H21), C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C23(H23A,H23B), C19(H19A,H19B), C20(H20A,H20B), C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C10(H10), C12(H12)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C2(H2A,H2B,H2C), C16(H16A,H16B,H16C), C3(H3A,H3B,H3C),
 C15(H15A,H15B,H15C)
;
_olex2_date_sample_data_collection 2018-09-12
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop in perfluoroether oil'
_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 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.927