Distinct Catalytic Performance of Dirhodium(II) Complexes with ortho-Metalated DPPP in Dehydrosilylation of Styrene Derivatives with Alkoxysilanes
Lu, Wenkui; Zhu, Xiaoyu; Yang, Liqun; Wu, Xiaoyu; Xie, Xiaomin; Zhang, Zhaoguo; ACS Catalysis 11 (2021) 10190–10197; doi:10.1021/acscatal.1c02129

data_4518936
_publ_section_title
;
 Distinct Catalytic Performance of Dirhodium(II) Complexes with
 ortho-Metalated DPPP in Dehydrosilylation of Styrene Derivatives with
 Alkoxysilanes
;
_journal_issue                   16
_journal_name_full               'ACS Catalysis'
_journal_page_first              10190
_journal_page_last               10197
_journal_paper_doi               10.1021/acscatal.1c02129
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C35 H36 N2 O4 P2 Rh2, 2(C2 H3 N)'
_chemical_formula_sum            'C39 H42 N4 O4 P2 Rh2'
_chemical_formula_weight         898.52
_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
_audit_creation_date             2021-01-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.967(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.358(3)
_cell_length_b                   10.6384(11)
_cell_length_c                   20.055(2)
_cell_measurement_reflns_used    9816
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.34
_cell_measurement_theta_min      2.99
_cell_volume                     3845.2(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60639
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.399
_diffrn_reflns_theta_min         2.993
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.093
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0820 before and 0.0565 after correction.
The Ratio of minimum to maximum transmission is 0.8515.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         7041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0211
_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^)+(0.0178P)^2^+3.4610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6283
_reflns_number_total             7041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c02129_si_003.cif
_cod_data_source_block           t_a
_cod_depositor_comments
'Adding full bibliography for 4518936--4518937.cif.'
_cod_database_code               4518936
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.498
_shelx_estimated_absorpt_t_min   0.294
_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 Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C20(H20), C19(H19), C17(H17), C24(H24), C26(H26), C25(H25),
 C15(H15), C2(H2), C11(H11), C18(H18), C6(H6), C14(H14), C12(H12), C5(H5),
 C3(H3), C4(H4), C13(H13)
2.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C33(H33A,H33B,H33C), C39(H39A,H39B,
 H39C), C31(H31A,H31B,H31C), C37(H37A,H37B,H37C)
;
_olex2_submission_special_instructions 'No special instructions were received'