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_7705755
_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 H34 N2 O Rh, B F4'
_chemical_formula_sum            'C24 H34 B F4 N2 O Rh'
_chemical_formula_weight         556.25
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2020-08-31 deposited with the CCDC.	2020-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 134.45(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.765(7)
_cell_length_b                   7.8159(6)
_cell_length_c                   24.836(4)
_cell_measurement_reflns_used    12326
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.1620
_cell_measurement_theta_min      3.5990
_cell_volume                     5787(3)
_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    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            48291
_diffrn_reflns_theta_full        25.217
_diffrn_reflns_theta_max         29.667
_diffrn_reflns_theta_min         2.982
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.823
_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            yellow
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.38
_refine_diff_density_min         -1.70
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9663
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         7538
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.0014441
_refine_ls_shift/su_mean         0.0000334
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 847. 0.130E+04 656. 156. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1115
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1115
_reflns_limit_h_max              40
_reflns_limit_h_min              -57
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                6591
_reflns_number_total             7556
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0622
_oxford_refine_ls_scale          1.127(3)
_oxford_reflns_number_all        7538
_cod_data_source_file            d0dt03698f2.cif
_cod_data_source_block           I_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7705753--7705755.cif.'
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               7705755
_oxdiff_exptl_absorpt_empirical_full_min 0.927
_oxdiff_exptl_absorpt_empirical_full_max 1.096
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_platon_squeeze_void_probe_radius 1.20