Ruthenium tris(σ-B-H) borate complexes: synthesis, structure, and reactivity
Wei, Yongliang; Yang, Xiaowen; Tian, Minghui; Wang, Xue; Wang, Tongdao; Dalton Transactions  (2022) –; doi:10.1039/D2DT03092F

data_7711383
_publ_section_title
;
 Ruthenium tris(\s-B-H) borate complexes: synthesis, structure, and
 reactivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03092F
_journal_year                    2022
_chemical_formula_moiety         'C24 H27 B Ru'
_chemical_formula_sum            'C24 H27 B Ru'
_chemical_formula_weight         427.33
_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             2022-09-14
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-22 deposited with the CCDC.	2022-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                114.054(7)
_cell_angle_beta                 99.367(7)
_cell_angle_gamma                104.778(8)
_cell_formula_units_Z            4
_cell_length_a                   11.932(3)
_cell_length_b                   13.828(4)
_cell_length_c                   14.862(4)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.671
_cell_measurement_theta_min      2.618
_cell_volume                     2064.0(10)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            53949
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.251
_diffrn_reflns_theta_min         2.617
_diffrn_source                   'sealed tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1129 before and 0.0673 after correction.
The Ratio of minimum to maximum transmission is 0.8985.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         10113
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0411P)^2^+0.3404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7500
_reflns_number_total             10113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03092f2.cif
_cod_data_source_block           3c
_cod_database_code               7711383
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.820
_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
 C39-C40 \\sim C39A-C40A
 with sigma of 0.02
 C39-C43 \\sim C39A-C43A
 with sigma of 0.02
 C39-C44 \\sim C39A-C44A
 with sigma of 0.02
 C40-C41 \\sim C40A-C41A
 with sigma of 0.02
 C40-C45 \\sim C40A-C45A
 with sigma of 0.02
 C41-C42 \\sim C41A-C42A
 with sigma of 0.02
 C41-C46 \\sim C41A-C46A
 with sigma of 0.02
 C42-C43 \\sim C42A-C43A
 with sigma of 0.02
 C42-C47 \\sim C42A-C47A
 with sigma of 0.02
 C43-C48 \\sim C43A-C48A
 with sigma of 0.02
 C39-C41 \\sim C39A-C41A
 with sigma of 0.04
 C39-C42 \\sim C39A-C42A
 with sigma of 0.04
 C39-C45 \\sim C39A-C45A
 with sigma of 0.04
 C39-C48 \\sim C39A-C48A
 with sigma of 0.04
 C39-Ru2 \\sim C39A-Ru2
 with sigma of 0.04
 C40-C42 \\sim C40A-C42A
 with sigma of 0.04
 C40-C43 \\sim C40A-C43A
 with sigma of 0.04
 C40-C44 \\sim C40A-C44A
 with sigma of 0.04
 C40-C46 \\sim C40A-C46A
 with sigma of 0.04
 C40-Ru2 \\sim C40A-Ru2
 with sigma of 0.04
 C41-C43 \\sim C41A-C43A
 with sigma of 0.04
 C41-C45 \\sim C41A-C45A
 with sigma of 0.04
 C41-C47 \\sim C41A-C47A
 with sigma of 0.04
 C41-Ru2 \\sim C41A-Ru2
 with sigma of 0.04
 C42-C46 \\sim C42A-C46A
 with sigma of 0.04
 C42-C48 \\sim C42A-C48A
 with sigma of 0.04
 C42-Ru2 \\sim C42A-Ru2
 with sigma of 0.04
 C43-C44 \\sim C43A-C44A
 with sigma of 0.04
 C43-C47 \\sim C43A-C47A
 with sigma of 0.04
 C43-Ru2 \\sim C43A-Ru2
 with sigma of 0.04
 C44-Ru2 \\sim C44A-Ru2
 with sigma of 0.04
 C45-Ru2 \\sim C45A-Ru2
 with sigma of 0.04
 C46-Ru2 \\sim C46A-Ru2
 with sigma of 0.04
 C47-Ru2 \\sim C47A-Ru2
 with sigma of 0.04
 C48-Ru2 \\sim C48A-Ru2
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C42A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C40A, C39A, C43A, C44A, C41A, C45A, C42A, C48A, C46A, C47A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, C39, C40, C43, C44, C41, C45, C42, C48, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C39A)=Sof(C40A)=Sof(C41A)=Sof(C42A)=Sof(C43A)=Sof(C44A)=Sof(H44D)=
 Sof(H44E)=Sof(H44F)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C46A)=
 Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=
 Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(1)
 Sof(C39)=Sof(C40)=Sof(C41)=Sof(C42)=Sof(C43)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(H44C)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C46)=Sof(H46A)=Sof(H46B)=
 Sof(H46C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48)=Sof(H48A)=Sof(H48B)=
 Sof(H48C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C34(H34), C35(H35),
  C36(H36), C37(H37)
6.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C44A(H44D,H44E,H44F),
 C45A(H45D,H45E,H45F), C46A(H46D,H46E,H46F), C47A(H47D,H47E,H47F), C48A(H48D,
 H48E,H48F)
;
_shelx_res_checksum              27823
_olex2_submission_special_instructions 'No special instructions were received'