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_7040261
_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         'C48 H43 N6 O P2 Ru, C24 H20 B'
_chemical_formula_sum            'C72 H63 B N6 O P2 Ru'
_chemical_formula_weight         1202.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-02-27
_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                 92.123(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.968(2)
_cell_length_b                   11.5676(7)
_cell_length_c                   28.5760(18)
_cell_measurement_reflns_used    5022
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.820
_cell_measurement_theta_min      2.811
_cell_volume                     12541.9(13)
_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      150.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.0000
_diffrn_reflns_av_unetI/netI     0.2546
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27324
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.042
_diffrn_reflns_theta_min         2.749
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1231 before and 0.0737 after correction.
The Ratio of minimum to maximum transmission is 0.8943.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       plate
_exptl_crystal_F_000             4992
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.363
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1524
_refine_ls_number_reflns         27320
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.1949
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0696P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11308
_reflns_number_total             27320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02459a2.cif
_cod_data_source_block           Compound_4
_cod_depositor_comments
'Adding full bibliography for 7040259--7040264.cif.'
_cod_original_cell_volume        12542.0(13)
_cod_database_code               7040261
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3E(0.046) H4E(0.057) H5E(0.061) H6EA(0.042) H6EB(0.042)
 H8E(0.052) H9E(0.055) H10E(0.046) H10F(0.046) H11E(0.063) H12A(0.045)
 H12B(0.047) H12E(0.065) H13A(0.052) H13B(0.052) H13E(0.06) H14A(0.056)
 H14B(0.068) H15A(0.057) H15B(0.082) H16A(0.041) H16B(0.064) H22A(0.058)
 H22B(0.041) H23A(0.073) H23B(0.054) H24A(0.063) H24B(0.055) H25A(0.055)
 H25B(0.052) H26A(0.043) H26B(0.038) H32A(0.05) H32B(0.04) H33A(0.065)
 H33B(0.05) H34A(0.067) H34B(0.054) H35A(0.059) H35B(0.048) H36A(0.043)
 H36B(0.042) H3G(0.044) H4G(0.054) H5G(0.043) H6GA(0.032) H6GB(0.032)
 H8G(0.046) H9G(0.044) H10A(0.044) H10B(0.044) H10C(0.044) H10D(0.044)
 H11'(0.071) H11G(0.063) H12'(0.081) H12C(0.039) H12D(0.033) H12G(0.066)
 H13'(0.056) H13C(0.055) H13D(0.039) H13G(0.054) H14C(0.05) H14D(0.047)
 H15C(0.047) H15D(0.045) H16C(0.035) H16D(0.039) H22C(0.033) H22D(0.043)
 H23C(0.044) H23D(0.05) H24C(0.044) H24D(0.049) H25C(0.043) H25D(0.045)
 H26C(0.033) H26D(0.036) H32C(0.041) H32D(0.037) H33C(0.049) H33D(0.042)
 H34C(0.06) H34D(0.049) H35C(0.051) H35D(0.043) H36C(0.05) H36D(0.037)
 H12M(0.052) H13M(0.06) H14M(0.064) H15M(0.067) H16M(0.058) H22M(0.063)
 H23M(0.072) H24M(0.076) H25M(0.07) H26M(0.057) H32M(0.042) H33M(0.046)
 H34M(0.051) H35M(0.054) H36M(0.048) H42M(0.062) H43M(0.073) H44M(0.063)
 H45M(0.065) H46M(0.05) H12N(0.038) H13N(0.044) H14N(0.056) H15N(0.054)
 H16N(0.043) H22N(0.037) H23N(0.05) H24N(0.05) H25N(0.05) H26N(0.045)
 H32N(0.043) H33N(0.05) H34N(0.056) H35N(0.052) H36N(0.041) H42N(0.036)
 H43N(0.049) H44N(0.046) H45N(0.04) H46N(0.034)
 Fixed X: H3E(0.6289) H4E(0.6929) H5E(0.7252) H6EA(0.6705) H6EB(0.7061)
 H8E(0.7052) H9E(0.6622) H10E(0.5745) H10F(0.5972) H11E(0.5428) H12A(0.5267)
 H12B(0.5476) H12E(0.5831) H13A(0.469) H13B(0.5078) H13E(0.6127) H14A(0.4565)
 H14B(0.4933) H15A(0.5008) H15B(0.5205) H16A(0.5581) H16B(0.5584) H22A(0.5635)
 H22B(0.6227) H23A(0.5811) H23B(0.6031) H24A(0.6358) H24B(0.5442) H25A(0.6734)
 H25B(0.5053) H26A(0.6552) H26B(0.524) H32A(0.6449) H32B(0.6604) H33A(0.6783)
 H33B(0.7138) H34A(0.6703) H34B(0.716) H35A(0.6284) H35B(0.6649) H36A(0.5972)
 H36B(0.6107) H3G(0.9013) H4G(0.8426) H5G(0.8013) H6GA(0.8469) H6GB(0.8091)
 H8G(0.8274) H9G(0.7955) H10A(0.9185) H10B(0.8882) H10C(0.8998) H10D(0.9205)
 H11'(0.8878) H11G(0.9514) H12'(0.8537) H12C(0.8514) H12D(0.872) H12G(0.896)
 H13'(0.8629) H13C(0.8011) H13D(0.8306) H13G(0.8699) H14C(0.8055) H14D(0.8263)
 H15C(0.8608) H15D(0.8658) H16C(0.9113) H16D(0.9067) H22C(0.8883) H22D(0.9593)
 H23C(0.9007) H23D(0.9561) H24C(0.9518) H24D(0.9143) H25C(0.9927) H25D(0.8767)
 H26C(0.9804) H26D(0.8806) H32C(0.9727) H32D(0.9961) H33C(1.0192) H33D(1.0508)
 H34C(1.0333) H34D(1.0554) H35C(1.0008) H35D(1.0054) H36C(0.9573) H36D(0.9489)
 H12M(0.7744) H13M(0.7427) H14M(0.7325) H15M(0.7535) H16M(0.7856) H22M(0.7508)
 H23M(0.7422) H24M(0.7874) H25M(0.8418) H26M(0.8509) H32M(0.77) H33M(0.7565)
 H34M(0.7742) H35M(0.8045) H36M(0.8186) H42M(0.8661) H43M(0.9257) H44M(0.9465)
 H45M(0.9077) H46M(0.8482) H12N(0.7648) H13N(0.773) H14N(0.7355) H15N(0.6916)
 H16N(0.6843) H22N(0.6604) H23N(0.6025) H24N(0.5831) H25N(0.6223) H26N(0.6795)
 H32N(0.7186) H33N(0.7567) H34N(0.8083) H35N(0.8221) H36N(0.783) H42N(0.7439)
 H43N(0.7473) H44N(0.7339) H45N(0.7187) H46N(0.7153)
 Fixed Y: H3E(0.6013) H4E(0.6109) H5E(0.5293) H6EA(0.3574) H6EB(0.4263)
 H8E(0.4837) H9E(0.5528) H10E(0.5898) H10F(0.6503) H11E(0.2685) H12A(0.3652)
 H12B(0.9251) H12E(0.3304) H13A(0.2944) H13B(0.996) H13E(0.51) H14A(0.1391)
 H14B(0.8918) H15A(0.053) H15B(0.7128) H16A(0.1238) H16B(0.6384) H22A(0.1509)
 H22B(0.8582) H23A(0.0751) H23B(0.945) H24A(0.123) H24B(0.9307) H25A(0.2451)
 H25B(0.8225) H26A(0.323) H26B(0.7378) H32A(0.1131) H32B(0.7106) H33A(0.0279)
 H33B(0.7961) H34A(0.0812) H34B(0.9313) H35A(0.2223) H35B(0.9787) H36A(0.3134)
 H36B(0.8951) H3G(0.9908) H4G(0.9887) H5G(0.8898) H6GA(0.7238) H6GB(0.785)
 H8G(0.9022) H9G(0.825) H10A(0.9799) H10B(1.0291) H10C(1.0426) H10D(0.9216)
 H11'(0.7694) H11G(0.6762) H12'(0.9639) H12C(1.0856) H12D(0.4974) H12G(0.7387)
 H13'(1.0768) H13C(1.1773) H13D(0.4126) H13G(0.8962) H14C(1.3136) H14D(0.4698)
 H15C(1.358) H15D(0.607) H16C(1.2708) H16D(0.692) H22C(1.2644) H22D(0.4979)
 H23C(1.355) H23D(0.4145) H24C(1.3135) H24D(0.4834) H25C(1.1852) H25D(0.6339)
 H26C(1.0903) H26D(0.717) H32C(1.2923) H32D(0.7421) H33C(1.363) H33D(0.6664)
 H34C(1.2754) H34D(0.5049) H35C(1.1166) H35D(0.4264) H36C(1.0378) H36D(0.5007)
 H12M(0.5129) H13M(0.4677) H14M(0.2752) H15M(0.1296) H16M(0.1757) H22M(0.2443)
 H23M(0.1264) H24M(0.0948) H25M(0.1826) H26M(0.2946) H32M(0.4481) H33M(0.6245)
 H34M(0.7965) H35M(0.7882) H36M(0.6128) H42M(0.5047) H43M(0.5086) H44M(0.3929)
 H45M(0.2721) H46M(0.269) H12N(0.5651) H13N(0.3842) H14N(0.2318) H15N(0.2614)
 H16N(0.4416) H22N(0.7703) H23N(0.7948) H24N(0.7182) H25N(0.6115) H26N(0.5802)
 H32N(0.761) H33N(0.7615) H34N(0.6518) H35N(0.5472) H36N(0.5442) H42N(0.8737)
 H43N(1.0409) H44N(1.0354) H45N(0.8593) H46N(0.6921)
 Fixed Z: H3E(0.5458) H4E(0.531) H5E(0.6002) H6EA(0.6619) H6EB(0.6749)
 H8E(0.7577) H9E(0.8119) H10E(0.7526) H10F(0.7942) H11E(0.8312) H12A(0.5948)
 H12B(0.6308) H12E(0.8973) H13A(0.596) H13B(0.5752) H13E(0.8702) H14A(0.6446)
 H14B(0.5081) H15A(0.6898) H15B(0.4971) H16A(0.6901) H16B(0.5538) H22A(0.5675)
 H22B(0.7175) H23A(0.4973) H23B(0.7844) H24A(0.4686) H24B(0.805) H25A(0.5122)
 H25B(0.7565) H26A(0.5825) H26B(0.6889) H32A(0.6403) H32B(0.6783) H33A(0.702)
 H33B(0.6602) H34A(0.7791) H34B(0.5995) H35A(0.7967) H35B(0.5575) H36A(0.736)
 H36B(0.5756) H3G(0.9836) H4G(1.0189) H5G(0.9601) H6GA(0.8858) H6GB(0.8825)
 H8G(0.7322) H9G(0.7995) H10A(0.7696) H10B(0.7344) H10C(0.7552) H10D(0.7577)
 H11'(0.62) H11G(0.6684) H12'(0.6021) H12C(0.8534) H12D(0.8915) H12G(0.6204)
 H13'(0.6714) H13C(0.8795) H13D(0.8401) H13G(0.6612) H14C(0.9399) H14D(0.762)
 H15C(0.9741) H15D(0.734) H16C(0.9469) H16D(0.7856) H22C(0.817) H22D(0.9327)
 H23C(0.7463) H23D(1.0066) H24C(0.7079) H24D(1.0585) H25C(0.7419) H25D(1.0352)
 H26C(0.8116) H26D(0.9622) H32C(0.8735) H32D(0.9055) H33C(0.9201) H33D(0.8898)
 H34C(0.9922) H34D(0.841) H35C(1.0164) H35D(0.8049) H36C(0.9666) H36D(0.8213)
 H12M(0.547) H13M(0.4783) H14M(0.4583) H15M(0.5082) H16M(0.5768) H22M(0.6457)
 H23M(0.7091) H24M(0.7653) H25M(0.756) H26M(0.6901) H32M(0.6978) H33M(0.7312)
 H34M(0.6965) H35M(0.6266) H36M(0.5947) H42M(0.6543) H43M(0.6379) H44M(0.5777)
 H45M(0.5368) H46M(0.5537) H12N(0.8271) H13N(0.7945) H14N(0.8125) H15N(0.865)
 H16N(0.8999) H22N(0.8516) H23N(0.873) H24N(0.9429) H25N(0.9897) H26N(0.9676)
 H32N(0.9802) H33N(1.0456) H34N(1.0462) H35N(0.9796) H36N(0.9153) H42N(0.9116)
 H43N(0.866) H44N(0.7864) H45N(0.7501) H46N(0.7956)
;
_shelx_res_checksum              14883
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'