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_7045477
_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     'C70 H58 N10 Na2 O12 Ru2, 4(C H4 O), 2(C2 H3 N)'
_chemical_formula_sum            'C78 H80 N12 Na2 O16 Ru2'
_chemical_formula_weight         1689.66
_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   mixed
_audit_creation_date             2017-12-18
_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                93.898(2)
_cell_angle_beta                 96.346(2)
_cell_angle_gamma                92.495(2)
_cell_formula_units_Z            1
_cell_length_a                   8.5931(7)
_cell_length_b                   12.6268(11)
_cell_length_c                   17.7433(15)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.53
_cell_volume                     1906.5(3)
_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      100.01
_diffrn_detector                 'Bruker PHOTON100 area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.0228
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28651
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.578
_diffrn_reflns_theta_min         2.316
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.483
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1351 before and 0.0365 after correction. The Ratio of minimum to maximum transmission is 0.9122. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         10644
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+1.8820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9700
_reflns_number_total             10644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03935b2.cif
_cod_data_source_block           emt-76
_cod_depositor_comments
;
Adding full bibliography for 7045471--7045478.cif.

2024-04-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C39 H40 N6 Na O8 Ru'
_cod_original_formula_weight         844.83
_cod_original_formula_moiety         'C35 H29 N5 Na O6 Ru, 2(C H4 O), C2 H3 N'
_cod_original_formula_units_Z            2
_cod_database_code               7045477
_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. Shared sites
{C009, N20}
{N00A, C14}
3. Restrained distances
 O007-H007
 0.87 with sigma of 0.01
 O013-C01G = O1-C8
 1.41 with sigma of 0.02
 H00M-O00G
 2.1 with sigma of 0.02
 C01I-H007
 1.895303 with sigma of 0.02
 Na00-H007
 2.892765 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C009) = Uanis(N20)
Uanis(N00A) = Uanis(C14)
5. Others
 Sof(O1)=Sof(H1)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=1-FVAR(1)
 Sof(O013)=Sof(H013)=Sof(C01G)=Sof(H01N)=Sof(H01O)=Sof(H01P)=FVAR(1)
 Fixed Sof: C009(0.5) N00A(0.5) H00A(0.5) H00F(0.5) H00B(0.5) H00J(0.5)
 C14(0.5) N20(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C00F(H00A), C00F(H00F), C00J(H00B), C00J(H00J), C00N(H00N), C00Q(H00Q),
 C00R(H00R), C00S(H00S), C00V(H00V), C00W(H00W), C00Z(H00Z), C011(H011),
 C012(H012), C015(H015), C016(H016), C017(H017), C018(H018), C01A(H01A),
 C01B(H01B), C01C(H01C), C01F(H01F)
6.b Idealised Me refined as rotating group:
 C01E(H01Q,H01R,H01S), C01G(H01N,H01O,H01P), C01H(H01D,H01E,H01G), C01I(H01H,
 H01I,H01J), C01J(H01K,H01L,H01M), C8(H8A,H8B,H8C)
6.c Idealised tetrahedral OH refined as rotating group:
 O00M(H00M), O013(H013), O1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'