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_7045474
_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         'C37 H32 N5 O4 Ru, C H2 Cl2, F6 P'
_chemical_formula_sum            'C38 H34 Cl2 F6 N5 O4 P Ru'
_chemical_formula_weight         941.64
_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             2017-12-18
_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                86.107(2)
_cell_angle_beta                 78.113(2)
_cell_angle_gamma                88.160(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2590(10)
_cell_length_b                   12.8556(14)
_cell_length_c                   17.920(2)
_cell_measurement_reflns_used    9312
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.250
_cell_measurement_theta_min      2.311
_cell_volume                     2082.1(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      100
_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 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23690
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.323
_diffrn_reflns_theta_min         2.248
_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    0.615
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1082 before and 0.0546 after correction. The Ratio of minimum to maximum transmission is 0.8017. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       plate
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
TITL emt-148_a.res in P-1
CELL    9.2590   12.8556   17.9200     86.11     78.11     88.16
SPGR P-1
C101 0.796 0.566 0.050 !       5.33 eA-3
C102 0.914 0.500 0.031 !       4.97 eA-3
C103 0.998 0.443 0.003 !       1.99 eA-3
Q104 0.660 0.225 0.231 !       1.58 eA-3
Q105 0.966 0.872 0.296 !       1.21 eA-3
Q106 0.601 0.194 0.318 !       1.19 eA-3
Q107 0.079 0.841 0.015 !       1.19 eA-3
Q108 0.380 0.558 0.120 !       1.03 eA-3
Q109 0.989 0.878 0.357 !       1.02 eA-3
Q110 0.695 0.160 0.270 !       1.00 eA-3
Q111 0.471 0.570 0.201 !       1.00 eA-3
Q112 0.451 0.591 0.233 !       0.92 eA-3
Q113 0.585 0.265 0.260 !       0.87 eA-3
Q114 0.090 0.954 0.138 !       0.78 eA-3
Q115 0.782 0.685 0.091 !       0.78 eA-3
Q116 0.672 0.549 0.079 !       0.76 eA-3
Q117 0.145 0.644 0.266 !       0.71 eA-3
Q118 0.873 0.102 0.009 !       0.71 eA-3
Q119 0.134 0.631 0.221 !       0.70 eA-3
Q120 0.368 0.488 0.248 !       0.69 eA-3
Q121 0.491 0.598 0.144 !       0.68 eA-3
Q122 0.331 0.424 0.015 !       0.67 eA-3
Q123 0.577 0.909 0.215 !       0.66 eA-3
Q124 0.160 0.614 0.175 !       0.66 eA-3
Q125 0.822 0.078 0.439 !       0.64 eA-3
Q126 0.737 0.500 0.111 !       0.64 eA-3
Q127 0.493 0.191 0.419 !       0.63 eA-3
Q128 0.383 0.201 0.438 !       0.62 eA-3
Q129 0.278 0.648 0.291 !       0.62 eA-3
Q130 0.204 0.492 0.046 !       0.62 eA-3
Q131 0.329 0.597 0.206 !       0.61 eA-3
Q132 0.530 0.324 0.047 !       0.60 eA-3
Q133 0.461 0.237 0.312 !       0.60 eA-3
Q134 0.272 0.488 0.301 !       0.60 eA-3
Q135 0.122 0.841 0.106 !       0.60 eA-3
Q136 0.556 0.119 0.468 !       0.59 eA-3
Q137 0.634 0.152 0.409 !       0.58 eA-3
Q138 0.555 0.312 0.140 !       0.58 eA-3
Q139 0.890 0.172 0.191 !       0.58 eA-3
Q140 0.413 0.190 0.395 !       0.58 eA-3
Q141 0.664 0.155 0.360 !       0.57 eA-3
Q142 0.180 0.047 0.362 !       0.57 eA-3
Q143 0.408 0.671 0.266 !       0.57 eA-3
Q144 0.276 0.490 0.216 !       0.56 eA-3
Q145 0.667 0.127 0.312 !       0.56 eA-3
Q146 0.094 0.424 0.064 !       0.56 eA-3
Q147 0.162 0.378 0.035 !       0.55 eA-3
Q148 0.606 0.216 0.376 !       0.55 eA-3
Q149 0.687 0.514 0.053 !       0.55 eA-3
Q150 0.847 0.037-0.002 !       0.55 eA-3
Q151 0.557 0.087 0.160 !       0.55 eA-3
Q152 0.904 0.334 0.250 !       0.54 eA-3
Q153 0.278 0.174 0.489 !       0.54 eA-3
Q154 0.557 0.285-0.003 !       0.54 eA-3
Q155 0.409 0.219 0.361 !       0.53 eA-3
Q156 0.292 0.719 0.157 !       0.52 eA-3
Q157 0.213 0.526 0.315 !       0.52 eA-3
Q158 0.752 0.123 0.344 !       0.52 eA-3
Q159 0.565 0.109 0.499 !       0.52 eA-3
Q160 0.627 0.014 0.470 !       0.51 eA-3
Q161 0.804 0.669 0.267 !       0.50 eA-3
Q162 0.268 0.654 0.403 !       0.50 eA-3
;
_refine_diff_density_max         1.171
_refine_diff_density_min         -1.300
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         9332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0570P)^2^+2.6855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7466
_reflns_number_total             9332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03935b2.cif
_cod_data_source_block           emt-148_sq
_cod_depositor_comments
'Adding full bibliography for 7045471--7045478.cif.'
_cod_database_code               7045474
_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
2.a Secondary CH2 refined with riding coordinates:
 C014(H01A,H01B), C01J(H01P,H01Q), C01K(H01K,H01L)
2.b Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00O(H00O), C00Q(H00Q), C00R(H00R), C00T(H00T), C00U(H00U),
 C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C012(H012), C013(H013),
 C015(H015), C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01C),
 C01B(H01D), C01G(H01H), C01H(H01I), C01I(H01J)
2.c Idealised Me refined as rotating group:
 C01C(H01E,H01F,H01G), C01L(H01M,H01N,H01O)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'