Insights into metal-ligand hydrogen transfer: a square-planar ruthenate complex supported by a tetradentate amino-amido-diolefin ligand
Demyan E. Prokopchuk; Alan J. Lough; Rafael E. Rodriguez-Lugo; Robert H. Morris; Hansjorg Grutzmacher; Chem.Commun. 52 (2016) 6138–; doi:

data_7119055
_publ_section_title
;
 Insights into metal-ligand hydrogen transfer: a square-planar ruthenate
 complex supported by a tetradentate amino-amido-diolefin ligand
;
_journal_name_full               Chem.Commun.
_journal_page_first              6138
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C72 H64 Cl4 N2 P2 Ru2'
_chemical_formula_sum            'C72 H64 Cl4 N2 P2 Ru2'
_chemical_formula_weight         1363.13
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-01-01 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                99.178(2)
_cell_angle_beta                 107.6360(10)
_cell_angle_gamma                97.263(2)
_cell_formula_units_Z            1
_cell_length_a                   10.3736(3)
_cell_length_b                   13.2432(4)
_cell_length_c                   13.7718(4)
_cell_measurement_temperature    100
_cell_volume                     1748.99(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34259
_diffrn_reflns_point_group_measured_fraction_full 0.915
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.926
_diffrn_reflns_theta_min         1.585
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_correction_T_min  0.7891
_exptl_absorpt_correction_type   ulti-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction.'
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       needle
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.078
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 6743 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         20628
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0519P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_full    0.831
_reflns_Friedel_fraction_max     0.717
_reflns_number_gt                17802
_reflns_number_total             20628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc00041j2.cif
_cod_data_source_block           Complex1
_cod_original_cell_volume        1748.98(9)
_cod_database_code               7119055
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Others
 Sof(C55B)=Sof(C56B)=Sof(H56B)=Sof(C58B)=Sof(H58B)=Sof(C59B)=Sof(H59B)=
 Sof(C60B)=Sof(H60B)=1-FVAR(1)
 Sof(C55A)=Sof(C56A)=Sof(H56A)=Sof(C58A)=Sof(H58A)=Sof(C59A)=Sof(H59A)=
 Sof(C60A)=Sof(H60A)=FVAR(1)
 Sof(C64B)=Sof(H64B)=Sof(C63B)=Sof(H63B)=Sof(C62B)=Sof(H62B)=Sof(C61B)=
 Sof(C66B)=Sof(H66B)=1-FVAR(2)
 Sof(C61A)=Sof(C62A)=Sof(H62A)=Sof(C63A)=Sof(H63A)=Sof(C64A)=Sof(H64A)=
 Sof(C66A)=Sof(H66A)=FVAR(2)
 Sof(C65B)=Sof(H65B)=1-FVAR(3)
 Sof(C65A)=Sof(H65A)=FVAR(3)
 Sof(C71B)=Sof(H71B)=Sof(C72B)=Sof(H72B)=Sof(C67B)=Sof(C68B)=Sof(H68B)=
 Sof(C69B)=Sof(H69B)=Sof(C70B)=Sof(H70B)=1-FVAR(4)
 Sof(C67A)=Sof(C68A)=Sof(H68A)=Sof(C69A)=Sof(H69A)=Sof(C70A)=Sof(H70A)=
 Sof(C71A)=Sof(H71A)=Sof(C72A)=Sof(H72A)=FVAR(4)
 Sof(P2B)=1-FVAR(5)
 Sof(P2A)=FVAR(5)
 Sof(C57B)=Sof(H57B)=1-FVAR(6)
 Sof(C57A)=Sof(H57A)=FVAR(6)
3.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), C1(H1A), C4(H4), C5(H5), C16(H16), C19(H19), C20(H20),
 C31(H31), C36(H36)
3.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15),
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45),
 C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54),
  C56A(H56A), C57A(H57A), C58A(H58A), C59A(H59A), C60A(H60A), C62A(H62A),
 C63A(H63A), C64A(H64A), C65A(H65A), C66A(H66A), C68A(H68A), C69A(H69A),
 C70A(H70A), C71A(H71A), C72A(H72A), C56B(H56B), C57B(H57B), C58B(H58B),
 C59B(H59B), C60B(H60B), C65B(H65B), C64B(H64B), C63B(H63B), C62B(H62B),
 C66B(H66B), C71B(H71B), C72B(H72B), C68B(H68B), C69B(H69B), C70B(H70B)
3.d Fitted hexagon refined as free rotating group:
 C65B(C64B,C63B,C62B,C61B,C66B), C71B(C72B,C67B,C68B,C69B,C70B)
;
_shelx_res_checksum              74216
_shelx_fab_checksum              46632
_olex2_submission_special_instructions 'No special instructions were received'