N^N^C-Cyclometalated rhodium(III) complexes with isomeric pyrimidine-based ligands: unveiling the impact of isomerism on structural motifs, luminescence and cytotoxicity.
Vorobyeva, Sofia N.; Bautina, Sof'ya A.; Shekhovtsov, Nikita A.; Nikolaenkova, Elena B.; Sukhikh, Taisiya S.; Golubeva, Yuliya A.; Klyushova, Lyubov S.; Krivopalov, Viktor P.; Rakhmanova, Marianna I.; Gourlaouen, Christophe; Bushuev, Mark B.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8398–8416; doi:10.1039/d4dt00824c

data_7715817
_publ_section_title
;
 N^N^C-Cyclometalated rhodium(III) complexes with isomeric
 pyrimidine-based ligands: unveiling the impact of isomerism on structural
 motifs, luminescence and cytotoxicity.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8398
_journal_page_last               8416
_journal_paper_doi               10.1039/d4dt00824c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C22.2 H21.4 Cl2 N4 O Rh, 0.4(C2 H6 O)'
_chemical_formula_sum            'C23 H23.8 Cl2 N4 O1.4 Rh'
_chemical_formula_weight         552.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-14 deposited with the CCDC.	2024-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                84.660(2)
_cell_angle_beta                 80.9050(10)
_cell_angle_gamma                79.224(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7080(3)
_cell_length_b                   9.5487(4)
_cell_length_c                   14.4311(6)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.66
_cell_measurement_theta_min      2.41
_cell_volume                     1161.47(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23075
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.684
_diffrn_reflns_theta_min         2.406
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             557
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         7138
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0330P)^2^+0.6596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5708
_reflns_number_total             7138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00824c2.cif
_cod_data_source_block           bsa-18
_cod_depositor_comments
'Adding full bibliography for 7715815--7715818.cif.'
_cod_database_code               7715817
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.890
_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. Shared sites
{O1B, O1A}
3. Restrained distances
 C23-C22 = C25-C24
 1.55 with sigma of 0.02
 O2-C24
 1.45 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O1B) = Uanis(O1A)
5. Rigid body (RIGU) restrains
 O1B, C23, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O1B)=Sof(O2)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=
 Sof(H25C)=1-FVAR(1)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(O1A)=
 FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B)
7.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C11(H11), C17(H17), C14(H14), C12(H12), C18(H18), C3(H3),
 C13(H13), C19(H19), C20(H20)
7.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              39830
_olex2_submission_special_instructions 'No special instructions were received'