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_7045472
_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(C32 H22 N6 O4 Ru), 2(Cl)'
_chemical_formula_sum            'C64 H44 Cl2 N12 O8 Ru2'
_chemical_formula_weight         1382.15
_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             2017-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-04-03 deposited with the CCDC.
2018-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                97.029(2)
_cell_angle_beta                 99.656(2)
_cell_angle_gamma                94.114(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7453(7)
_cell_length_b                   13.6624(7)
_cell_length_c                   19.9377(10)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.414
_cell_measurement_theta_min      2.113
_cell_volume                     3381.7(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      99.98
_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 0.997
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12420
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.414
_diffrn_reflns_theta_max         25.414
_diffrn_reflns_theta_min         2.113
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.745212
_exptl_absorpt_correction_T_min  0.701973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Twinabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       prism
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
TITL emt-twin5 P -1         R = 0.10
CELL   12.7453   13.6624   19.9377     97.03     99.66     94.11
SPGR P-1
C101 0.971 0.707 0.377 !       5.17 eA-3
C102 0.591 0.198 0.169 !       4.34 eA-3
C103 0.892 0.462 0.104 !       4.26 eA-3
C104 0.281 0.041 0.499 !       4.03 eA-3
C105 0.235 0.146 0.348 !       3.95 eA-3
C106 0.050 0.256 0.311 !       3.71 eA-3
C107 0.377 0.065 0.486 !       3.29 eA-3
C108 0.097 0.348 0.215 !       3.14 eA-3
C109 0.345 0.146 0.481 !       3.05 eA-3
C110 0.489 0.242 0.177 !       2.88 eA-3
C111 0.959 0.436 0.069 !       2.71 eA-3
C112 0.965 0.341 0.098 !       2.61 eA-3
C113 0.535 0.301 0.112 !       2.50 eA-3
C114 0.471 0.259 0.224 !       2.32 eA-3
C115 0.984 0.406 0.093 !       2.23 eA-3
C116 0.395 0.232 0.157 !       1.98 eA-3
C117 0.281 0.249 0.252 !       1.86 eA-3
C118 0.410 0.808 0.159 !       1.72 eA-3
C119 0.169 0.280 0.237 !       1.66 eA-3
C120 0.234 0.224 0.295 !       1.65 eA-3
C121 0.154 0.255 0.279 !       1.62 eA-3
Q122 0.692 0.289 0.047 !       1.32 eA-3
C123 0.094 0.287 0.254 !       1.32 eA-3
C124 0.453 0.696 0.215 !       1.24 eA-3
C125 0.393 0.206 0.201 !       1.24 eA-3
Q126 0.801 0.309 0.082 !       1.14 eA-3
C127 0.170 0.205 0.325 !       1.11 eA-3
Q128 0.122 0.876 0.308 !       1.03 eA-3
C129 0.358 0.294 0.204 !       1.01 eA-3
C130 0.373 0.246 0.213 !       0.97 eA-3
Q131 0.606 0.014 0.094 !       0.92 eA-3
Q132 0.737 0.828 0.430 !       0.90 eA-3
C133 0.200 0.258 0.190 !       0.85 eA-3
C134 0.267 0.317 0.234 !       0.84 eA-3
Q135 0.814 0.438 0.488 !       0.77 eA-3
Q136 0.496 0.097 0.317 !       0.77 eA-3
C137 0.269 0.191 0.470 !       0.77 eA-3
C138 0.341 0.225 0.244 !       0.76 eA-3
Q139 0.487 0.512 0.301 !       0.75 eA-3
C140 0.059 0.777 0.387 !       0.75 eA-3
Q141 0.405 0.333 0.211 !       0.75 eA-3
Q142 0.640 0.510 0.208 !       0.75 eA-3
Q143 0.512 0.308 0.483 !       0.73 eA-3
Q144 0.313 0.016 0.158 !       0.73 eA-3
Q145 0.184 0.958 0.324 !       0.72 eA-3
Q146 0.468 0.889 0.101 !       0.71 eA-3
C147 0.514 0.167 0.156 !       0.70 eA-3
Q148 0.450 0.086 0.449 !       0.68 eA-3
Q149 0.512 0.887 0.062 !       0.68 eA-3
Q150 0.891 0.849 0.309 !       0.67 eA-3
Q151 0.027 0.406 0.187 !       0.67 eA-3
Q152 0.701 0.956 0.112 !       0.67 eA-3
Q153 0.499 0.879 0.018 !       0.67 eA-3
Q154 0.827 0.452 0.442 !       0.66 eA-3
Q155 0.250 0.863 0.279 !       0.66 eA-3
Q156 0.505 0.982 0.066 !       0.65 eA-3
Q157 0.752 0.329 0.114 !       0.65 eA-3
Q158 0.764 0.762 0.388 !       0.64 eA-3
Q159 0.673 0.684 0.234 !       0.64 eA-3
Q160 0.966 0.736 0.438 !       0.64 eA-3
Q161 0.450 0.435 0.278 !       0.63 eA-3
Q162 0.143 0.937 0.173 !       0.63 eA-3
Q163 0.799 0.407 0.269 !       0.63 eA-3
Q164 0.285 0.510 0.327 !       0.63 eA-3
Q165 0.412 0.470 0.356 !       0.63 eA-3
Q166 0.658 0.615 0.222 !       0.62 eA-3
Q167 0.298 0.054 0.140 !       0.61 eA-3
Q168 0.655 0.008 0.357 !       0.61 eA-3
Q169 0.924 0.931 0.062 !       0.60 eA-3
Q170 0.695 0.559 0.074 !       0.60 eA-3
Q171 0.297 0.801 0.448 !       0.60 eA-3
Q172 0.982 0.719 0.068 !       0.60 eA-3
Q173 0.529 0.836 0.033 !       0.60 eA-3
Q174 0.280 0.966 0.092 !       0.59 eA-3
Q175 0.607 0.667 0.204 !       0.59 eA-3
Q176 0.595 0.398 0.343 !       0.59 eA-3
Q177 0.425 0.122 0.142 !       0.59 eA-3
Q178 0.765 0.239 0.406 !       0.58 eA-3
Q179 0.658 0.501 0.140 !       0.58 eA-3
Q180 0.188 0.019 0.372 !       0.58 eA-3
Q181 0.017 0.504 0.091 !       0.57 eA-3
Q182 0.762 0.356 0.220 !       0.57 eA-3
Q183 0.232 0.943 0.200 !       0.57 eA-3
C184 0.370 0.039 0.422 !       0.57 eA-3
C185 0.469 0.335 0.121 !       0.57 eA-3
C186 0.064 0.239 0.220 !       0.57 eA-3
Q187 0.044 0.600 0.264 !       0.57 eA-3
Q188 0.674 0.704 0.331 !       0.56 eA-3
Q189 0.983 0.289 0.125 !       0.56 eA-3
Q190 0.308 0.300 0.329 !       0.56 eA-3
Q191 0.973 0.702 0.125 !       0.56 eA-3
Q192 0.702 0.559 0.103 !       0.56 eA-3
Q193 0.659 0.460 0.160 !       0.56 eA-3
Q194 0.781 0.095 0.390 !       0.56 eA-3
Q195 0.467 0.487 0.269 !       0.56 eA-3
C196 0.456 0.779 0.218 !       0.56 eA-3
Q197 0.284 0.995 0.296 !       0.56 eA-3
C198 0.108 0.147 0.311 !       0.56 eA-3
C199 0.500 1.000 0.500 !       0.56 eA-3
;
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         12420
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0683
_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^)+(0.0231P)^2^+6.9328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10055
_reflns_number_total             12420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03935b2.cif
_cod_data_source_block           emt-twin5_sq-1
_cod_depositor_comments
'Adding full bibliography for 7045471--7045478.cif.'
_cod_database_code               7045472
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5541(11) 0.4459(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid body (RIGU) restrains
 C11, C14, C10, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C0AA, C8, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O01E(0.5) O01K(0.5) O01M(0.5) C025(0.75) H025(0.75) C02A(0.5)
 H02A(0.5) C02B(0.75) H02B(0.75) C02E(0.75) H02E(0.75) C02H(0.75) H02H(0.75)
 C5(0.5) H5(0.5) C7(0.5) H7(0.5) C9(0.5) H9(0.5) C10(0.25) H10(0.25) C12(0.25)
 H12(0.25) C14(0.25) H14(0.25) C8(0.5) H8(0.5) C0AA(0.5) H0AA(0.5) C11(0.25)
 H11(0.25) C19(0.5) H19(0.5) O10(0.5) O18(0.5) O2(0.5) O6(0.5) C20(0.5)
 H20(0.5) O0AA(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00P(H00P), C00R(H00R), C00U(H00U), C00W(H00W), C00X(H00X),
 C00Y(H00Y), C010(H010), C011(H011), C014(H014), C015(H015), C016(H016),
 C017(H017), C018(H018), C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D),
 C01G(H01G), C01H(H01H), C01J(H01J), C01O(H01O), C01Q(H01Q), C01R(H01R),
 C01S(H01S), C01U(H01U), C01V(H01V), C01X(H01X), C01Y(H01Y), C021(H021),
 C022(H022), C023(H023), C025(H025), C026(H026), C027(H027), C029(H029),
 C02A(H02A), C02B(H02B), C02D(H02D), C02E(H02E), C02H(H02H), C5(H5), C7(H7),
 C9(H9), C10(H10), C12(H12), C14(H14), C8(H8), C0AA(H0AA), C11(H11), C19(H19),
 C20(H20)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'