Ruthenium(ii) complexes of hemilabile pincer ligands: synthesis and catalysing the transfer hydrogenation of ketones.
Nair, Ashwin G.; McBurney, Roy T.; Walker, D. Barney; Page, Michael J.; Gatus, Mark R. D.; Bhadbhade, Mohan; Messerle, Barbara A.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 14335–14342; doi:10.1039/c6dt02459a

data_7040263
_publ_section_title
;
 Ruthenium(ii) complexes of hemilabile pincer ligands: synthesis and
 catalysing the transfer hydrogenation of ketones.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14335
_journal_page_last               14342
_journal_paper_doi               10.1039/c6dt02459a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C21 H26 Cl N6 Ru, B5 H4 O10'
_chemical_formula_sum            'C21 H30 B5 Cl N6 O10 Ru'
_chemical_formula_weight         717.08
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-20 deposited with the CCDC.
2016-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.366(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3903(4)
_cell_length_b                   11.8757(4)
_cell_length_c                   23.6462(9)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    150.04
_cell_measurement_theta_max      27.005
_cell_measurement_theta_min      2.455
_cell_volume                     3135.84(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.04
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27698
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.029
_diffrn_reflns_theta_min         1.862
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1317 before and 0.0450 after correction.
The Ratio of minimum to maximum transmission is 0.8857.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'yellowish orange'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.058
_refine_diff_density_max         1.100
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         6823
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+1.7077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5718
_reflns_number_total             6823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02459a2.cif
_cod_data_source_block           p21byn_a
_cod_depositor_comments
'Adding full bibliography for 7040259--7040264.cif.'
_cod_database_code               7040263
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O9-H9 = O4-H4 = O3AA-H3AA
 0.9 with sigma of 0.02
 B2-H4 \\sim B5-H9 \\sim H3AA-B3
 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C8D(H8D)
3.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C1AA(H1AA,H1AB)
3.c Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1C(H1C), C2A(H2A), C2B(H2B), C2C(H2C), C2D(H2D), C3A(H3A),
 C3B(H3B), C3C(H3C), C3D(H3D), C5D(H5D), C6D(H6D)
3.d Idealised Me refined as rotating group:
 C7D(H7DA,H7DB,H7DC), C9D(H9DA,H9DB,H9DC), C10D(H10A,H10B,H10C)
3.e Idealised tetrahedral OH refined as rotating group:
 O10(H10)
;
_shelx_res_checksum              40378
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'