Selective dehydrogenation of ammonia borane to polycondensated BN rings catalysed by ruthenium olefin complexes.
Himmelbauer, Daniel; Müller, Fabian; Schweinzer, Clara; Casas, Fernando; Pribanic, Bruno; Le Corre, Grégoire; Thöny, Debora; Trincado, Monica; Grützmacher, Hansjörg; Chemical communications (Cambridge, England) 60 (2024) 885–888; doi:10.1039/d3cc05709g

data_7132504
_publ_section_title
;
 Selective dehydrogenation of ammonia borane to polycondensated BN rings
 catalysed by ruthenium olefin complexes.
;
_journal_issue                   7
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              885
_journal_page_last               888
_journal_paper_doi               10.1039/d3cc05709g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C64 H52 N4 Ru2, 3(C4 H8 O)'
_chemical_formula_sum            'C76 H76 N4 O3 Ru2'
_chemical_formula_weight         1295.54
_chemical_name_systematic        '[Ru2(trop2dae)(trop2dad)]x3(THF)'
_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   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc28s6cn
_audit_creation_date             2021-09-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-11-19 deposited with the CCDC.	2023-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.9100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.47460(10)
_cell_length_b                   23.4500(2)
_cell_length_c                   23.6481(2)
_cell_measurement_reflns_used    44039
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6730
_cell_measurement_theta_min      1.7360
_cell_volume                     5805.44(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -62.35 143.40   0.25   89.93    --  -23.61  73.75-130.74  823
  2  \w    -62.35 143.40   0.25   89.93    --  -23.61  73.75  76.26  823
  3  \w    -62.35 143.40   0.25   89.93    --  -23.61  73.75 -25.74  823
  4  \w    -62.35 143.40   0.25   89.93    --  -23.61  73.75  25.26  823
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0394262000
_diffrn_orient_matrix_UB_12      0.0158703000
_diffrn_orient_matrix_UB_13      0.0192335000
_diffrn_orient_matrix_UB_21      -0.0538363000
_diffrn_orient_matrix_UB_22      0.0061464000
_diffrn_orient_matrix_UB_23      0.0163601000
_diffrn_orient_matrix_UB_31      0.0117295000
_diffrn_orient_matrix_UB_32      -0.0250146000
_diffrn_orient_matrix_UB_33      0.0162061000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            81371
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.723
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.16b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         11859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+8.4570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9857
_reflns_number_total             11859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05709g2.cif
_cod_data_source_block           finalrun074
_cod_depositor_comments          'Adding full bibliography for 7132504.cif.'
_cod_database_code               7132504
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C76H76N4O3Ru2
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.824
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Others
 Sof(H75C)=Sof(H75D)=Sof(C76B)=Sof(H76C)=Sof(H76D)=1-FVAR(1)
 Sof(H75A)=Sof(H75B)=Sof(C76A)=Sof(H76A)=Sof(H76B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), C52(H52), C51(H51), C5(H5), C37(H37), C36(H36), C4(H4),
 C63(H63), C33(H33), C48(H48), C16(H16), C1(H1A), C64(H64)
4.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C31(H31A,H31B), C72(H72A,H72B), C69(H69A,H69B), C71(H71A,
 H71B), C70(H70A,H70B), C74(H74A,H74B), C65(H65A,H65B), C66(H66A,H66B),
 C67(H67A,H67B), C75(H75A,H75B), C75(H75C,H75D), C68(H68A,H68B), C76A(H76A,
 H76B), C73(H73A,H73B), C76B(H76C,H76D)
4.c Aromatic/amide H refined with riding coordinates:
 C62(H62), C15(H15), C40(H40), C42(H42), C11(H11), C55(H55), C12(H12),
 C57(H57), C56(H56), C61(H61), C10(H10), C43(H43), C41(H41), C60(H60), C19(H19),
  C23(H23), C58(H58), C14(H14), C8(H8), C59(H59), C47(H47), C13(H13), C20(H20),
 C26(H26), C44(H44), C30(H30), C46(H46), C45(H45), C9(H9), C25(H25), C24(H24),
 C29(H29), C27(H27), C28(H28)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.061
_oxdiff_exptl_absorpt_empirical_full_min 0.947