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_7040259
_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
'2(C22 H24 Ag N12), C22 H23 Ag N12, 3(C24 H20 B)'
_chemical_formula_sum            'C138 H131 Ag3 B3 N36'
_chemical_formula_weight         2649.82
_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             2015-02-26
_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                99.448(2)
_cell_angle_beta                 99.315(2)
_cell_angle_gamma                106.299(2)
_cell_formula_units_Z            2
_cell_length_a                   14.4586(6)
_cell_length_b                   19.1802(7)
_cell_length_c                   24.5632(10)
_cell_measurement_reflns_used    8293
_cell_measurement_temperature    149.99
_cell_measurement_theta_max      22.384
_cell_measurement_theta_min      2.509
_cell_volume                     6291.9(4)
_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      149.99
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.0841
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            87774
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.134
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1562 before and 0.0674 after correction.
The Ratio of minimum to maximum transmission is 0.9281.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       plate
_exptl_crystal_F_000             2734
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1624
_refine_ls_number_reflns         21420
_refine_ls_number_restraints     482
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13558
_reflns_number_total             21420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02459a2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 7040259--7040264.cif.'
_cod_database_code               7040259
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A1(0.051) H1A2(0.063) H1C1(0.085) H1C2(0.057) H1PA(0.042)
 H1PB(0.042) H1PC(0.043) H1PD(0.043) H2A1(0.055) H2A2(0.085) H2B1(0.036)
 H2B2(0.037) H2C1(0.084) H2C2(0.068) H2PA(0.036) H2PB(0.036) H2PC(0.039)
 H2PD(0.039) H3A1(0.043) H3A2(0.065) H3B1(0.033) H3B2(0.035) H3C1(0.069)
 H3C2(0.056) H1A5(0.06) H1C5(0.112) H1RA(0.049) H1RB(0.049) H2A5(0.051)
 H2B5(0.063) H2C5(0.11) H2RA(0.054) H2RB(0.054) H3A5(0.044) H3B5(0.073)
 H3C5(0.082) H1A3(0.049) H1A4(0.052) H1C3(0.097) H1C4(0.103) H1Q(0.04)
 H1QA(0.04) H1QB(0.04) H2A3(0.052) H2A4(0.058) H2B3(0.048) H2B4(0.048)
 H2C3(0.084) H2C4(0.107) H2QA(0.036) H2QB(0.036) H2QC(0.045) H2QD(0.045)
 H3A3(0.047) H3A4(0.054) H3B3(0.043) H3B4(0.048) H3C3(0.063) H3C4(0.073)
 H1A6(0.043) H1C6(0.064) H1SA(0.039) H1SB(0.039) H2A6(0.051) H2B6(0.036)
 H2C6(0.067) H2SA(0.036) H2SB(0.036) H3A6(0.044) H3B6(0.036) H3C6(0.053)
 H12M(0.028) H13M(0.034) H14M(0.039) H15M(0.037) H16M(0.027) H22M(0.041)
 H23M(0.064) H24M(0.078) H25M(0.075) H26M(0.047) H32M(0.037) H33M(0.045)
 H34M(0.04) H35M(0.038) H36M(0.029) H42M(0.032) H43M(0.039) H44M(0.042)
 H45M(0.043) H46M(0.035) H12O(0.038) H13O(0.055) H14O(0.067) H15O(0.056)
 H16O(0.034) H22O(0.034) H23O(0.042) H24O(0.043) H25O(0.035) H26O(0.029)
 H32O(0.028) H33O(0.032) H34O(0.035) H35O(0.034) H36O(0.03) H42O(0.031)
 H43O(0.038) H44O(0.039) H45O(0.034) H46O(0.03) H12N(0.032) H13N(0.036)
 H14N(0.04) H15N(0.037) H16N(0.033) H22N(0.038) H23N(0.052) H24N(0.061)
 H25N(0.053) H26N(0.04) H32N(0.038) H33N(0.045) H34N(0.045) H35N(0.038)
 H36N(0.031) H42N(0.028) H43N(0.035) H44N(0.039) H45N(0.037) H46N(0.03)
 Fixed X: H1A1(-0.0787) H1A2(0.3945) H1C1(0.1033) H1C2(0.2847) H1PA(0.2461)
 H1PB(0.2464) H1PC(0.0746) H1PD(0.0382) H2A1(-0.1024) H2A2(0.3491) H2B1(0.3075)
 H2B2(0.0465) H2C1(-0.0135) H2C2(0.3749) H2PA(0.2675) H2PB(0.3381) H2PC(0.0159)
 H2PD(0.0703) H3A1(0.065) H3A2(0.1741) H3B1(0.3423) H3B2(0.0379) H3C1(0.0767)
 H3C2(0.2587) Ag1C(0) H1A5(-0.2599) H1C5(0.4252) H1RA(-0.1431) H1RB(-0.1385)
 H2A5(-0.2563) H2B5(0.0178) H2C5(0.3352) H2RA(0.2101) H2RB(0.2718) H3A5(-
 0.1769) H3B5(0.1932) H3C5(0.2217) H1A3(0.5817) H1A4(0.0851) H1C3(-0.0932)
 H1C4(0.7486) H1Q(0.4645) H1QA(0.1571) H1QB(0.166) H2A3(0.5862) H2A4(0.096)
 H2B3(0.2929) H2B4(0.3132) H2C3(-0.0033) H2C4(0.6604) H2QA(0.0456) H2QB(0.1113)
 H2QC(0.5287) H2QD(0.5802) H3A3(0.503) H3A4(0.1515) H3B3(0.1209) H3B4(0.4916)
 H3C3(0.1048) H3C4(0.5414) Ag1D(0.5) H1A6(0.2624) H1C6(0.4023) H1SA(0.5924)
 H1SB(0.5888) H2A6(0.2539) H2B6(0.6146) H2C6(0.2841) H2SA(0.5677) H2SB(0.638)
 H3A6(0.421) H3B6(0.6248) H3C6(0.3765) H12M(0.299) H13M(0.4102) H14M(0.3604)
 H15M(0.1959) H16M(0.0866) H22M(-0.0201) H23M(-0.1829) H24M(-0.2736) H25M(-
 0.2034) H26M(-0.0436) H32M(0.1255) H33M(0.1517) H34M(0.1718) H35M(0.1663)
 H36M(0.1382) H42M(-0.0226) H43M(0.0068) H44M(0.1684) H45M(0.2996) H46M(0.2692)
 H12O(0.6537) H13O(0.8136) H14O(0.9424) H15O(0.9097) H16O(0.7498) H22O(0.6798)
 H23O(0.6629) H24O(0.526) H25O(0.4036) H26O(0.4208) H32O(0.5802) H33O(0.4751)
 H34O(0.3165) H35O(0.2664) H36O(0.3717) H42O(0.55) H43O(0.5423) H44O(0.5287)
 H45O(0.5177) H46O(0.5292) H12N(0.9693) H13N(1.0966) H14N(1.0675) H15N(0.9111)
 H16N(0.7862) H22N(0.7164) H23N(0.5678) H24N(0.4243) H25N(0.4293) H26N(0.577)
 H32N(0.636) H33N(0.6351) H34N(0.7675) H35N(0.9027) H36N(0.9008) H42N(0.7947)
 H43N(0.8154) H44N(0.8265) H45N(0.8183) H46N(0.7961)
 Fixed Y: H1A1(-0.2719) H1A2(-0.057) H1C1(0.1771) H1C2(-0.479) H1PA(-0.1003)
 H1PB(-0.1575) H1PC(-0.153) H1PD(-0.2042) H2A1(-0.1814) H2A2(-0.122)
 H2B1(0.0355) H2B2(-0.3428) H2C1(0.0597) H2C2(-0.3598) H2PA(-0.0204)
 H2PB(0.0617) H2PC(-0.3992) H2PD(-0.3159) H3A1(-0.0896) H3A2(-0.2009)
 H3B1(0.1057) H3B2(-0.4258) H3C1(-0.0348) H3C2(-0.2856) Ag1C(0.5) H1A5(0.2882)
 H1C5(0.4047) H1RA(0.4486) H1RB(0.4904) H2A5(0.2098) H2B5(0.4498) H2C5(0.346)
 H2RA(0.5484) H2RB(0.5785) H3A5(0.2996) H3B5(0.4924) H3C5(0.4194) H1A3(0.3714)
 H1A4(-0.0719) H1C3(0.3) H1C4(0.0785) H1Q(0.2055) H1QA(0.0852) H1QB(0.1282)
 H2A3(0.4644) H2A4(-0.1493) H2B3(0.2525) H2B4(0.0807) H2C3(0.3447) H2C4(0.021)
 H2QA(0.1169) H2QB(0.1401) H2QC(0.2209) H2QD(0.2421) H3A3(0.3911) H3A4(-0.0604)
 H3B3(0.2159) H3B4(0.1371) H3C3(0.2646) H3C4(0.0914) Ag1D(0.5) H1A6(0.3837)
 H1C6(0.8455) H1SA(0.5607) H1SB(0.5075) H2A6(0.4499) H2B6(0.6965) H2C6(0.7252)
 H2SA(0.6496) H2SB(0.7317) H3A6(0.5439) H3B6(0.772) H3C6(0.6335) H12M(0.1372)
 H13M(0.0713) H14M(-0.0448) H15M(-0.0954) H16M(-0.0292) H22M(0.0369) H23M(-
 0.0416) H24M(-0.0757) H25M(-0.0275) H26M(0.0543) H32M(0.0702) H33M(0.1302)
 H34M(0.2572) H35M(0.3231) H36M(0.2626) H42M(0.1649) H43M(0.2464) H44M(0.3105)
 H45M(0.2866) H46M(0.2026) H12O(0.3542) H13O(0.417) H14O(0.3728) H15O(0.2586)
 H16O(0.1924) H22O(0.2238) H23O(0.1508) H24O(0.044) H25O(0.0147) H26O(0.0883)
 H32O(0.3489) H33O(0.4204) H34O(0.3761) H35O(0.2606) H36O(0.1896) H42O(0.2472)
 H43O(0.1875) H44O(0.0607) H45O(-0.004) H46O(0.0573) H12N(0.4967) H13N(0.4463)
 H14N(0.3343) H15N(0.2763) H16N(0.3284) H22N(0.3055) H23N(0.2233) H24N(0.2552)
 H25N(0.3709) H26N(0.4537) H32N(0.4367) H33N(0.5064) H34N(0.6134) H35N(0.6479)
 H36N(0.578) H42N(0.6085) H43N(0.6757) H44N(0.6189) H45N(0.4932) H46N(0.4264)
 Fixed Z: H1A1(0.3386) H1A2(0.6841) H1C1(0.569) H1C2(0.4368) H1PA(0.3329)
 H1PB(0.3736) H1PC(0.595) H1PD(0.6375) H2A1(0.2794) H2A2(0.7601) H2B1(0.3824)
 H2B2(0.6166) H2C1(0.5753) H2C2(0.4138) H2PA(0.5749) H2PB(0.5781) H2PC(0.42)
 H2PD(0.4156) H3A1(0.2916) H3A2(0.7238) H3B1(0.4805) H3B2(0.5264) H3C1(0.5706)
 H3C2(0.41) Ag1C(1) H1A5(0.9482) H1C5(1.1276) H1RA(1.1421) H1RB(1.0908)
 H2A5(1.0203) H2B5(1.1995) H2C5(1.0273) H2RA(1.0561) H2RB(1.1202) H3A5(1.1135)
 H3B5(1.1927) H3C5(1.0022) H1A3(1.0599) H1A4(0.9266) H1C3(0.8974) H1C4(1.1273)
 H1Q(0.8708) H1QA(1.1197) H1QB(1.0693) H2A3(0.999) H2A4(0.9982) H2B3(0.8068)
 H2B4(1.1813) H2C3(0.9977) H2C4(1.0276) H2QA(0.8865) H2QB(0.9497) H2QC(1.0632)
 H2QD(1.1291) H3A3(0.901) H3A4(1.0919) H3B3(0.8204) H3B4(1.1874) H3C3(1.0142)
 H3C4(1.0047) Ag1D(1.5) H1A6(1.3424) H1C6(1.5701) H1SA(1.3472) H1SB(1.3912)
 H2A6(1.2641) H2B6(1.3852) H2C6(1.574) H2SA(1.5797) H2SB(1.5826) H3A6(1.2792)
 H3B6(1.4787) H3C6(1.5717) H12M(1.3108) H13M(1.3014) H14M(1.2378) H15M(1.1882)
 H16M(1.1969) H22M(1.1568) H23M(1.1271) H24M(1.1943) H25M(1.2901) H26M(1.3194)
 H32M(1.3618) H33M(1.4551) H34M(1.4792) H35M(1.4074) H36M(1.3136) H42M(1.1854)
 H43M(1.126) H44M(1.123) H45M(1.1779) H46M(1.2353) H12O(0.7178) H13O(0.7126)
 H14O(0.741) H15O(0.7678) H16O(0.7688) H22O(0.8451) H23O(0.9112) H24O(0.8948)
 H25O(0.8122) H26O(0.7465) H32O(0.8033) H33O(0.8071) H34O(0.7489) H35O(0.6864)
 H36O(0.6807) H42O(0.6342) H43O(0.5432) H44O(0.5232) H45O(0.5956) H46O(0.6872)
 H12N(1.3346) H13N(1.328) H14N(1.264) H15N(1.2047) H16N(1.2092) H22N(1.2895)
 H23N(1.2955) H24N(1.2816) H25N(1.2627) H26N(1.2574) H32N(1.174) H33N(1.1055)
 H34N(1.1133) H35N(1.1908) H36N(1.2593) H42N(1.3218) H43N(1.4123) H44N(1.4895)
 H45N(1.473) H46N(1.3823)
;
_shelx_res_checksum              78698
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'