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_7705754
_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 N2 O Rh'
_chemical_formula_sum            'C24 H33 N2 O Rh'
_chemical_formula_weight         468.43
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   32.883(3)
_cell_length_b                   32.883(3)
_cell_length_c                   10.4799(11)
_cell_measurement_reflns_used    5048
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.4280
_cell_measurement_theta_min      3.3980
_cell_volume                     9813.7(16)
_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_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.872
_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  0.062
_diffrn_reflns_av_unetI/netI     0.070
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            16712
_diffrn_reflns_theta_full        26.472
_diffrn_reflns_theta_max         29.615
_diffrn_reflns_theta_min         3.230
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.785
_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)

;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4392
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.184
_refine_diff_density_max         2.14
_refine_diff_density_min         -2.43
_refine_ls_extinction_coef       880(90)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9704
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         5332
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.0002778
_refine_ls_shift/su_mean         0.0000201
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.10P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2150
_refine_ls_wR_factor_gt          0.1854
_refine_ls_wR_factor_ref         0.2150
_reflns_limit_h_max              21
_reflns_limit_h_min              -42
_reflns_limit_k_max              45
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                4430
_reflns_number_total             5342
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.73
_oxford_diffrn_Wilson_scale      7.11
_oxford_refine_ls_r_factor_ref   0.0910
_oxford_refine_ls_scale          0.922(8)
_oxford_reflns_number_all        5332
_cod_data_source_file            d0dt03698f2.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7705753--7705755.cif.
;
_cod_original_cell_volume        9813.7(19)
_cod_original_sg_symbol_H-M      'R -3 '
_cod_database_code               7705754
_oxdiff_exptl_absorpt_empirical_full_min 0.859
_oxdiff_exptl_absorpt_empirical_full_max 1.424
_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)