Adaptability of the SiNN Pincer Ligand in Iridium and Rhodium Complexes Relevant to Borylation Catalysis
Lee, Chun-I; Hirscher, Nathanael A.; Zhou, Jia; Bhuvanesh, Nattamai; Ozerov, Oleg V.; Organometallics 34 (2015) 3099–; doi:10.1021/acs.organomet.5b00125

data_4085871
_publ_section_title
;
 Adaptability of the SiNN Pincer Ligand in Iridium and Rhodium Complexes
 Relevant to Borylation Catalysis
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3099
_journal_paper_doi               10.1021/acs.organomet.5b00125
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C35 H52 B2 N2 O4 Rh Si'
_chemical_formula_sum            'C35 H52 B2 N2 O4 Rh Si'
_chemical_formula_weight         717.40
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-01-13
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.157(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.013(2)
_cell_length_b                   18.428(3)
_cell_length_c                   18.279(3)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.037
_cell_measurement_theta_min      2.211
_cell_volume                     3905.8(11)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41033
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.640
_diffrn_reflns_theta_min         2.075
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0758 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.7817.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'yellowish green'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.352
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         8171
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+3.4397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6628
_reflns_number_total             8171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00125_si_002.cif
_cod_data_source_block           3b-Rh
_cod_depositor_comments
'Adding full bibliography for 4085870--4085871.cif.'
_cod_original_cell_volume        3905.6(12)
_cod_database_code               4085871
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.864
_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. Shared sites
{C31, C31A}
3. Restrained distances
 C35A-C31A \\sim C35-C31 \\sim C34A-C31A \\sim C34-C31
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C31) = Uanis(C31A)
5. Others
 Sof(C31A)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35A)=Sof(H35D)=
 Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(C31)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C8(H8), C12(H12), C13(H13), C15(H15)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C34A(H34D,H34E,
 H34F), C35A(H35D,H35E,H35F)
;
_shelx_res_checksum              491
_shelx_hkl_checksum              43746
_shelx_fab_checksum              42536