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_7040264
_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         'C11 H13 N6, C24 H20 B'
_chemical_formula_sum            'C35 H33 B N6'
_chemical_formula_weight         548.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-05-20 deposited with the CCDC.
2016-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5977(3)
_cell_length_b                   17.9211(6)
_cell_length_c                   19.1642(7)
_cell_measurement_reflns_used    6247
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.974
_cell_measurement_theta_min      2.509
_cell_volume                     2952.82(18)
_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  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 0.994
_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  0.0509
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14308
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_min         3.113
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1486 before and 0.0706 after correction.
The Ratio of minimum to maximum transmission is 0.7217.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.459
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.149
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 2160 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+0.4490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1049
_reflns_Friedel_coverage         0.732
_reflns_Friedel_fraction_full    0.968
_reflns_number_gt                5658
_reflns_number_total             6260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02459a2.cif
_cod_data_source_block           p212121_a
_cod_depositor_comments
'Adding full bibliography for 7040259--7040264.cif.'
_cod_database_code               7040264
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C1A(H1AA), C1B(H1BA), C1C(H1C), C2A(H2AA), C2B(H2BA), C2C(H2C), C3A(H3A),
 C3B(H3B), C3C(H3C), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
;
_shelx_res_checksum              70772
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'