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_7045471
_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         'C25 H22 N5 Ru, F6 P, C2 H3 N'
_chemical_formula_sum            'C27 H25 F6 N6 P Ru'
_chemical_formula_weight         679.57
_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                102.363(2)
_cell_angle_beta                 107.081(2)
_cell_angle_gamma                94.071(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5477(10)
_cell_length_b                   12.2940(13)
_cell_length_c                   12.7589(13)
_cell_measurement_reflns_used    9368
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.50
_cell_measurement_theta_min      2.36
_cell_volume                     1383.9(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      100.15
_diffrn_detector                 'Bruker PHOTON100 area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.995
_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  0.0215
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 0.995
_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       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            45870
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.502
_diffrn_reflns_theta_min         2.255
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1107 before and 0.0366 after correction. The Ratio of minimum to maximum transmission is 0.8822. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       prism
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.921
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         9149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+1.1937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8722
_reflns_number_total             9149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03935b2.cif
_cod_data_source_block           emt-ru-mecn2_a_pl
_cod_depositor_comments
'Adding full bibliography for 7045471--7045478.cif.'
_cod_database_code               7045471
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C17(H17), C6(H6), C15(H15), C21(H21), C16(H16), C7(H7),
 C3(H3), C9(H9), C5(H5), C8(H8), C20(H20), C18(H18), C4(H4), C19(H19)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C)
;
_olex2_submission_special_instructions 'No special instructions were received'