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_7045478
_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(C37 H32 N5 O4 Ru), 2(F6 P), C3 H6 O'
_chemical_formula_sum            'C77 H70 F12 N10 O9 P1.98 Ru2'
_chemical_formula_weight         1770.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 92.5090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5215(8)
_cell_length_b                   29.5909(15)
_cell_length_c                   18.0996(10)
_cell_measurement_reflns_used    9102
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.35
_cell_volume                     8305.1(8)
_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      100.02
_diffrn_detector                 'Bruker PHOTON100 area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            178386
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.555
_diffrn_reflns_theta_min         2.181
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1455 before and 0.0507 after correction. The Ratio of minimum to maximum transmission is 0.9166. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             3598
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1071
_refine_ls_number_reflns         25404
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0401P)^2^+6.8121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21223
_reflns_number_total             25404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03935b2.cif
_cod_data_source_block           emt74sq_sq
_cod_depositor_comments
'Adding full bibliography for 7045471--7045478.cif.'
_cod_database_code               7045478
_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. Restrained distances
 P004-F00V \\sim P004-F00W
 with sigma of 0.02
 P004-F01R \\sim P004-F01S
 with sigma of 0.02
 P004-F032 \\sim P004-F0
 with sigma of 0.02
 P004-F11 \\sim P004-F11A \\sim P004-F007
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O00N, C033, C039
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O00N, C9, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P004, F01R, F032, F010, F007, F00V, F11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P004, F0, F11A, F010, F007, F00W, F01S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: F00V(0.6) F01R(0.6) F032(0.6) C033(0.6) H03A(0.6) H03B(0.6)
 C039(0.6) H03C(0.6) H03D(0.6) H03E(0.6) F11(0.6) C1(0.4) H1A(0.4) H1B(0.4)
 H1C(0.4) C9(0.4) H9A(0.4) H9B(0.4) F0(0.4) F11A(0.4) F01S(0.4) F00W(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C02T(H02S,H02T), C02U(H02A,H02D), C030(H03F,H03G), C033(H03A,H03B), C9(H9A,H9B)
5.b Aromatic/amide H refined with riding coordinates:
 C013(H013), C014(H014), C01A(H01A), C01B(H01B), C01C(H01C), C01E(H01E),
 C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L),
 C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01S(H01S), C01T(H01T),
 C01V(H01V), C01W(H01W), C01Z(H01Z), C021(H021), C022(H022), C023(H023),
 C024(H024), C026(H026), C027(H027), C028(H028), C029(H029), C02B(H02B),
 C02C(H02C), C02E(H02M), C02G(H02G), C02H(H02N), C02I(H02I), C02J(H02J),
 C02K(H02K), C02L(H02L), C02M(H02O), C02O(H02P), C02P(H02Q), C02R(H02R),
 C02V(H02V), C02W(H02W)
5.c Idealised Me refined as rotating group:
 C02Q(H02Z,H,HA), C02S(H02,HB,HC), C02Y(H02U,H02X,H02Y), C02Z(H02E,H02F,H02H),
 C034(H03H,H03I,H03J), C039(H03C,H03D,H03E), C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'