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_7711380
_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         '1(C19 H29 B Ru)'
_chemical_formula_sum            'C19 H29 B Ru'
_chemical_formula_weight         369.30
_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   mixed
_audit_creation_date             2022-09-15
_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                90
_cell_angle_beta                 97.2870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.5721(3)
_cell_length_b                   7.85900(10)
_cell_length_c                   27.1629(4)
_cell_measurement_reflns_used    7438
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      27.495
_cell_measurement_theta_min      2.337
_cell_volume                     3720.88(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.00
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.957
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            17923
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.503
_diffrn_reflns_theta_min         1.470
_diffrn_source                   'sealed tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.068
_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     545
_refine_ls_number_reflns         8180
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0237P)^2^+2.3944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6766
_reflns_number_total             8180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03092f2.cif
_cod_data_source_block           3a
_cod_database_code               7711380
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.759
_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
 Ru2-C29 \\sim Ru2-C30 \\sim Ru2-C31 \\sim Ru2-C32 \\sim Ru2-C33
 with sigma of 0.02
 C29-C30 \\sim C30-C31 \\sim C31-C32 \\sim C32-C33
 with sigma of 0.02
 C29-C34 \\sim C30-C35 \\sim C31-C36 \\sim C32-C37 \\sim C33-C38
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C20 \\sim B2 \\sim Ru2 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim
C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim B2A \\sim Ru2A \\sim C29A
\\sim C30A \\sim C31A \\sim C32A \\sim C33A \\sim C34A \\sim C35A \\sim C36A
\\sim C37A \\sim C38A: within 0.9A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 0.9A
Uanis(Ru2) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq,
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(B2A) \\sim Ueq, Uanis(Ru2A) \\sim Ueq, Uanis(C29A) \\sim Ueq,
Uanis(C30A) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C32A) \\sim Ueq,
Uanis(C33A) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C35A) \\sim Ueq,
Uanis(C36A) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C38A) \\sim Ueq: with sigma
of 0.007 and sigma for terminal atoms of 0.014
Uanis(B2) \\sim Ueq, Uanis(B2A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Sof(B2A)=Sof(Ru2A)=Sof(C29A)=Sof(C30A)=Sof(C31A)=Sof(C32A)=Sof(C33A)=
 Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C37A)=Sof(H37D)=
 Sof(H37E)=Sof(H37F)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(H2AA)=
 Sof(H2AB)=Sof(H2AC)=1-FVAR(1)
 Sof(B2)=Sof(Ru2)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(C32)=Sof(C33)=Sof(C34)=
 Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=
 Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=
 Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C24(H24), C22(H22)
5.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C),
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C34A(H34D,H34E,H34F), C35A(H35D,H35E,H35F), C36A(H36D,
 H36E,H36F), C37A(H37D,H37E,H37F), C38A(H38D,H38E,H38F)
;
_shelx_res_checksum              33826
_olex2_submission_special_instructions 'No special instructions were received'