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_7045473
_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
'C31.94 H22.13 N4.9 O4 Ru, C H4 O, C0.9 H3.47 O0.9, 0.1(C11 H8 N)'
_chemical_formula_sum            'C34.9 H30.38 N5 O5.9 Ru'
_chemical_formula_weight         715.32
_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             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                90
_cell_angle_beta                 100.516(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5773(10)
_cell_length_b                   12.7565(9)
_cell_length_c                   17.9162(12)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.346
_cell_measurement_theta_min      2.619
_cell_volume                     3050.9(4)
_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      99.99
_diffrn_detector                 'Bruker PHOTON100 area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_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       '\f and \w scans'
_diffrn_radiation_collimation    'Rh-coated Si focusing mirrors'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.370
_diffrn_reflns_theta_min         2.360
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Wiggler, Station I911-3, MAX II, MAXLAB'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0827 before and 0.0430 after correction. The Ratio of minimum to maximum transmission is 0.8770. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.053
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7597
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0691P)^2^+2.6404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6141
_reflns_number_total             7597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03935b2.cif
_cod_data_source_block           emt-114_a
_cod_depositor_comments
'Adding full bibliography for 7045471--7045478.cif.'
_cod_original_formula_sum        'C34.90 H30.38 N5 O5.90 Ru'
_cod_database_code               7045473
_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-H1
 1.81 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uiso(C28) = Uiso(C5) = Uiso(C0) = Uiso(C3AA) = Uiso(C2AA) = Uiso(C9)
Uiso(C5AA) = Uiso(C6AA) = Uiso(C16) = Uiso(N29) = Uiso(C1AA) = Uiso(C4)
Uiso(C7) = Uiso(C0AA) = Uiso(C11) = Uiso(N8)
4. Others
 1*[Sof(O014)+Sof(H014)]+1*[Sof(O1)]=0.9 with esd of 0.0001
 Sof(N8)=Sof(C0AA)=Sof(C7)=Sof(H7)=Sof(C11)=Sof(H11)=Sof(H00A)=Sof(H00B)=
 Sof(C5)=Sof(C28)=Sof(C9)=Sof(H9)=Sof(C2AA)=Sof(H2AA)=Sof(C3AA)=Sof(H3AA)=
 Sof(C0)=Sof(H0)=Sof(C1AA)=Sof(C4)=Sof(H4)=Sof(C5AA)=Sof(H5AA)=Sof(C6AA)=
 Sof(H6AA)=Sof(C16)=Sof(H16)=Sof(N29)=Sof(H1)=1-FVAR(1)
 Sof(N007)=Sof(N009)=Sof(C00C)=Sof(C00R)=Sof(C00S)=Sof(C00U)=Sof(H00U)=
 Sof(C00V)=Sof(H00V)=Sof(C00W)=Sof(H00W)=Sof(C00X)=Sof(C00Y)=Sof(H00Y)=
 Sof(H8AA)=Sof(C010)=Sof(H010)=Sof(C011)=Sof(H011)=Sof(C012)=Sof(H012)=
 Sof(C015)=Sof(H015)=Sof(C016)=Sof(H016)=Sof(C017)=Sof(H017)=Sof(H00Q)=
 Sof(H00P)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(1)
 Sof(O014)=Sof(H014)=FVAR(2)
5.a Free rotating group:
 O1(H1)
5.b Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00H(H00H), C00K(H00K), C00M(H00M), C00N(H00N), C00O(H00O),
 C00U(H00U), C00V(H00V), C00W(H00W), C00Y(H00Y), C8AA(H8AA), C010(H010),
 C011(H011), C012(H012), C013(H013), C015(H015), C016(H016), C017(H017),
 C018(H018), C019(H019), C7(H7), C11(H11), C00Q(H00Q), C00Q(H00A), C00P(H00P),
 C00P(H00B), C9(H9), C2AA(H2AA), C3AA(H3AA), C0(H0), C4(H4), C5AA(H5AA),
 C6AA(H6AA), C16(H16)
5.c Fitted hexagon refined as free rotating group:
 N8(C0AA,C7,C11,C00Q,C00P), C5(C28,C9,C2AA,C3AA,C0), C1AA(C4,C5AA,C6AA,C16,N29)
5.d Idealised Me refined as rotating group:
 C01A(H01A,H01B,H01C), C1(H1A,H1B,H1C)
5.e Idealised tetrahedral OH refined as rotating group:
 O003(H003), O00B(H00C), O014(H014)
;
_olex2_submission_special_instructions 'No special instructions were received'