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_7040262
_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
'4(C17 H18 Cl N6 Ru), 2.5(C H4 O), 4(C24 H20 B), 1.5(O)'
_chemical_formula_sum            'C166.5 H162 B4 Cl4 N24 O4 Ru4'
_chemical_formula_weight         3152.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_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                74.808(4)
_cell_angle_beta                 89.916(4)
_cell_angle_gamma                81.797(4)
_cell_formula_units_Z            2
_cell_length_a                   16.8274(12)
_cell_length_b                   18.3619(15)
_cell_length_c                   24.387(2)
_cell_measurement_reflns_used    6652
_cell_measurement_temperature    150.01
_cell_measurement_theta_max      22.07
_cell_measurement_theta_min      4.38
_cell_volume                     7192.3(10)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.1205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25306
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         0.866
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1176 before and 0.0739 after correction.
The Ratio of minimum to maximum transmission is 0.8562.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       plate
_exptl_crystal_F_000             3250
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.045
_refine_diff_density_max         4.690
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1863
_refine_ls_number_reflns         25306
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1364
_refine_ls_R_factor_gt           0.0889
_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^)+(0.0789P)^2^+83.1282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2086
_refine_ls_wR_factor_ref         0.2371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16497
_reflns_number_total             25306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02459a2.cif
_cod_data_source_block           p1bar
_cod_depositor_comments
'Adding full bibliography for 7040259--7040264.cif.'
_cod_original_cell_volume        7192.5(10)
_cod_original_formula_sum        'C166.50 H162 B4 Cl4 N24 O4 Ru4'
_cod_database_code               7040262
_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. Rigid body (RIGU) restrains
 N5L, C8L
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: O2AA(0.5) O5AA(0.5) O3AA(0.5) O1(0.5) H1(0.5) C5(0.5) H5A(0.5)
 H5B(0.5) H5C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C4F(H4FA,H4FB), C8F(H8FA,H8FB), C4H(H4HA,H4HB), C8H(H8HA,H8HB), C4J(H4JA,
 H4JB), C8J(H8JA,H8JB), C4L(H4LA,H4LB), C8L(H8LA,H8LB)
4.b Aromatic/amide H refined with riding coordinates:
 C1E(H1E), C2E(H2E), C3E(H3E), C4E(H4E), C5E(H5E), C6E(H6E), C1F(H1F),
 C2F(H2F), C3F(H3F), C5F(H5F), C6F(H6F), C9F(H9F), C10F(H10F), C11F(H11F),
 C1G(H1G), C2G(H2G), C3G(H3G), C4G(H4G), C5G(H5G), C6G(H6G), C1H(H1H), C2H(H2H),
  C3H(H3H), C5H(H5H), C6H(H6H), C9H(H9H), C10H(H10H), C11H(H11H), C1I(H1I),
 C2I(H2I), C3I(H3I), C4I(H4I), C5I(H5I), C6I(H6I), C1J(H1J), C2J(H2J), C3J(H3J),
  C5J(H5J), C6J(H6J), C9J(H9J), C10J(H10J), C11J(H11J), C1K(H1K), C2K(H2K),
 C3K(H3K), C4K(H4K), C5K(H5K), C6K(H6K), C1L(H1L), C2L(H2L), C3L(H3L), C5L(H5L),
  C6L(H6L), C9L(H9L), C10L(H10L), C11L(H11L), C33D(H33D), C45C(H45C),
 C45B(H45B), C45D(H45D), C13C(H13C), C33C(H33C), C25C(H25C), C12A(H12A),
 C13D(H13D), C14A(H14A), C25D(H25D), C15A(H15A), C16A(H16A), C43B(H43B),
 C22A(H22A), C15C(H15C), C23A(H23A), C23C(H23C), C24A(H24A), C25A(H25A),
 C35C(H35C), C26A(H26A), C43C(H43C), C32A(H32A), C15D(H15D), C33A(H33A),
 C23D(H23D), C34A(H34A), C35A(H35A), C35D(H35D), C36A(H36A), C43D(H43D),
 C42B(H42B), C42A(H42A), C44B(H44B), C43A(H43A), C46B(H46B), C44A(H44A),
 C12C(H12C), C45A(H45A), C14C(H14C), C46A(H46A), C16C(H16C), C22C(H22C),
 C24C(H24C), C26C(H26C), C32C(H32C), C12B(H12B), C34C(H34C), C13B(H13B),
 C36C(H36C), C14B(H14B), C42C(H42C), C15B(H15B), C44C(H44C), C16B(H16B),
 C46C(H46C), C12D(H12D), C22B(H22B), C14D(H14D), C23B(H23B), C16D(H16D),
 C24B(H24B), C22D(H22D), C25B(H25B), C24D(H24D), C26B(H26B), C26D(H26D),
 C32D(H32D), C32B(H32B), C34D(H34D), C33B(H33B), C36D(H36D), C34B(H34B),
 C42D(H42D), C35B(H35B), C44D(H44D), C36B(H36B), C46D(H46D), C13A(H13A)
4.c Idealised Me refined as rotating group:
 C4AA(H4AA,H4AB,H4AC), C5AA(H5AA,H5AB,H5AC), C5(H5A,H5B,H5C)
4.d Idealised tetrahedral OH refined as rotating group:
 O0AA(H0AA), O1AA(H1AA), O1(H1)
;
_shelx_res_checksum              77870
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'