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_7711384
_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         'C37 H44 B P Ru'
_chemical_formula_sum            'C37 H44 B P Ru'
_chemical_formula_weight         631.57
_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     direct
_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                85.50
_cell_angle_beta                 88.45
_cell_angle_gamma                69.31
_cell_formula_units_Z            2
_cell_length_a                   9.61760(10)
_cell_length_b                   10.06670(10)
_cell_length_c                   17.7082(2)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      32.928
_cell_measurement_theta_min      2.264
_cell_volume                     1598.95(3)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.00
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.794
_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  0.0143
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.794
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15972
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.928
_diffrn_reflns_theta_min         2.168
_diffrn_source                   'sealed tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6672
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.065
_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     381
_refine_ls_number_reflns         9529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0273P)^2^+0.8788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8868
_reflns_number_total             9529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03092f2.cif
_cod_data_source_block           4b
_cod_database_code               7711384
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.863
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27),
 C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36),
  C37(H37)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C)
;
_shelx_res_checksum              30423
_olex2_submission_special_instructions 'No special instructions were received'