Cyclometalated ruthenium complexes with carboxylated ligands from a combined experimental/computational perspective.
Thoresen, Eirik Mydske; Balcells, David; Øien-Ødegaard, Sigurd; Hylland, Knut Tormodssønn; Tilset, Mats; Amedjkouh, Mohamed; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2589–2601; doi:10.1039/c7dt03935b

data_7045476
_publ_section_title
;
 Cyclometalated ruthenium complexes with carboxylated ligands from a
 combined experimental/computational perspective.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2589
_journal_page_last               2601
_journal_paper_doi               10.1039/c7dt03935b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '2(C37 H32 N5 O4 Ru), 2(F6 P), C H4 O'
_chemical_formula_sum            'C75 H64 F12 N10 O9 P2 Ru2'
_chemical_formula_weight         1741.44
_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             2017-12-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-20 deposited with the CCDC.
2018-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                82.510(2)
_cell_angle_beta                 67.804(2)
_cell_angle_gamma                81.017(2)
_cell_formula_units_Z            1
_cell_length_a                   11.3476(7)
_cell_length_b                   12.5085(8)
_cell_length_c                   13.5994(9)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      2.39
_cell_volume                     1760.0(2)
_computing_cell_refinement       'APEX3 (Bruker AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker AXS, 2016)'
_computing_data_reduction        'APEX3 (Bruker AXS, 2016)'
_computing_molecular_graphics    'Diamond v4 (Brandenburg, 2012)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.04
_diffrn_detector                 'Bruker PHOTON100 area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture, CMOS detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45114
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.385
_diffrn_reflns_theta_min         2.224
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0661 before and 0.0467 after correction. The Ratio of minimum to maximum transmission is 0.9517. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       prism
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         7179
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0223P)^2^+1.3641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6093
_reflns_number_total             7179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03935b2.cif
_cod_data_source_block           emt-ru-deeb
_cod_depositor_comments
'Adding full bibliography for 7045471--7045478.cif.'
_cod_database_code               7045476
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 C1-O0AA
 1.41 with sigma of 0.02
 C3-O2
 1.41 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C1)
4. Others
 Sof(O6)=Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=1-
 FVAR(1)
 Sof(O018)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C4AA)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=
 FVAR(1)
 Fixed Sof: O0AA(0.25) H0AA(0.25) O2(0.25) H2(0.25) C3(0.25) H3A(0.25)
 H3B(0.25) H3C(0.25) C1(0.25) H1A(0.25) H1B(0.25) H1C(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C01G(H01H,H01I), C3AA(H3AA,H3AB), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00N(H00N), C00P(H00P), C00R(H00R), C00T(H00T), C00U(H00U),
 C00V(H00V), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011),
 C012(H012), C013(H013), C014(H014), C015(H015), C017(H017), C019(H019),
 C01A(H01A), C01B(H01B), C01D(H01D), C01E(H01E)
5.c Idealised Me refined as rotating group:
 C01F(H01C,H01F,H01G), C4AA(H4AA,H4AB,H4AC), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C),
 C1(H1A,H1B,H1C)
5.d Idealised tetrahedral OH refined as rotating group:
 O0AA(H0AA), O2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'