Distinct modes of Si–H binding to Rh in complexes of a phosphine-diarylamido-silane (SiNP) pincer ligand
Rain Talosig, A.; Cosio, Mario N.; Morse, Benjamin; Nguyen, Vinh T.; Kosanovich, Alex J.; Pell, Christopher J.; Li, Chun; Bhuvanesh, Nattamai; Zhou, Jia; Larsen, Anna S.; Ozerov, Oleg. V.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02175G

data_7711110
_publ_section_title
;
 Distinct modes of Si--H binding to Rh in complexes of a
 phosphine-diarylamido-silane (SiNP) pincer ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02175G
_journal_year                    2022
_chemical_formula_moiety         'C29 H50 N O3 P2 Rh Si'
_chemical_formula_sum            'C29 H50 N O3 P2 Rh Si'
_chemical_formula_weight         653.64
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-24 deposited with the CCDC.	2022-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                103.562(7)
_cell_angle_beta                 105.146(8)
_cell_angle_gamma                100.236(8)
_cell_formula_units_Z            4
_cell_length_a                   12.957(4)
_cell_length_b                   14.254(4)
_cell_length_c                   19.296(5)
_cell_measurement_reflns_used    9023
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.396
_cell_measurement_theta_min      2.156
_cell_volume                     3233.8(16)
_computing_cell_refinement
'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.'
_computing_data_reduction
'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.'
_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_temperature      110.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker PHOTON'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34328
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.610
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0739 before and 0.0567 after correction. The Ratio of minimum to maximum transmission is 0.9150. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.182
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         11373
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0283P)^2^+1.6050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8389
_reflns_number_total             11373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02175g3.cif
_cod_data_source_block           mc328
_cod_original_cell_volume        3233.8(15)
_cod_database_code               7711110
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.846
_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. Restrained distances
 C25-C24 \\sim C26A-C24A \\sim C26-C24 \\sim C25A-C24A
 with sigma of 0.02
 Si1-C24A \\sim Si1-C24
 with sigma of 0.02
 Si1-C21 \\sim Si1-C21A
 with sigma of 0.02
 C22A-C21A \\sim C23-C21 \\sim C23A-C21A \\sim C22-C21
 with sigma of 0.02
 P2-O3 \\sim P2-O3A
 with sigma of 0.02
 O3A-C29A \\sim O3-C29
 with sigma of 0.02
 Si1B-H1B \\sim Si1-H1
 with sigma of 0.02
 Rh1-H1 \\sim Rh1B-H1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C24 \\sim C25 \\sim C26 \\sim C24A \\sim C25A \\sim C26A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C21 \\sim C22 \\sim C23 \\sim C21A \\sim C22A \\sim C23A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.04
O3 \\sim C29 \\sim O3A \\sim C29A \\sim P2: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C24) = Uanis(C24A)
Uanis(C21) = Uanis(C21A)
Uanis(C22A) = Uanis(C23A) = Uanis(C22)
4. Rigid body (RIGU) restrains
 C24, C25, C26, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C21, C22, C23, C21A, C22A, C23A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 P2, O3, C29, O3A, C29A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
5. Others
 Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23A)=
 Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25D)=
 Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(O3A)=Sof(C29A)=
 Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=
 Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(O3)=Sof(C29)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C21(H21), C21A(H21A), C24(H24), C24A(H24A), C15B(H15B),
 C18B(H18B), C21B(H21B), C24B(H24B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C3B(H3B), C5B(H5B),
 C6B(H6B), C9B(H9B), C10B(H10B), C12B(H12B)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C22A(H22D,H22E,H22F), C23A(H23D,H23E,H23F), C25(H25A,H25B,H25C),
 C26(H26A,H26B,H26C), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C29A(H29D,H29E,H29F),
 C7B(H7BA,H7BB,H7BC), C14B(H14D,H14E,H14F), C16B(H16D,H16E,H16F), C17B(H17D,
 H17E,H17F), C19B(H19D,H19E,H19F), C20B(H20D,H20E,H20F), C22B(H22G,H22H,H22I),
 C23B(H23G,H23H,H23I), C25B(H25G,H25H,H25I), C26B(H26G,H26H,H26I), C27B(H27D,
 H27E,H27F), C28B(H28D,H28E,H28F), C29B(H29G,H29H,H29I)
;
_shelx_res_checksum              73851
_olex2_submission_special_instructions 'No special instructions were received'