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_7715816
_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         'C21.646 H20.292 Cl2 N4 O Rh, 0.677(C2 H6 O)'
_chemical_formula_sum            'C23 H24.35 Cl2 N4 O1.67 Rh'
_chemical_formula_weight         557.43
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-13 deposited with the CCDC.	2024-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                103.5000(10)
_cell_angle_beta                 92.4590(10)
_cell_angle_gamma                91.6840(10)
_cell_formula_units_Z            2
_cell_length_a                   8.8156(3)
_cell_length_b                   10.9113(4)
_cell_length_c                   12.2108(5)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.31
_cell_volume                     1140.11(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0295
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14266
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.558
_diffrn_reflns_theta_min         2.256
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0585 before and 0.0456 after correction.
The Ratio of minimum to maximum transmission is 0.8020.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             566
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6959
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0328P)^2^+0.1183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5684
_reflns_number_total             6959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00824c2.cif
_cod_data_source_block           u
_cod_depositor_comments
'Adding full bibliography for 7715815--7715818.cif.'
_cod_database_code               7715816
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.872
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2A,H2B,H2C} of C2, {H7A,H7B,H7C} of C7, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, {H25A,H25B,H25C} of C25, {H23A,H23B,H23C} of C23, All O(H,
  H) groups
2. Restrained distances
 H1B-O1 \\sim O1-H1A
 with sigma of 0.02
3. Others
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=1-FVAR(1)
 Sof(O2)=Sof(H2)=Sof(H1B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C24)=
 Sof(H24A)=Sof(H24B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C22(H22A,H22B)
4.b Me refined with riding coordinates:
 C25(H25A,H25B,H25C), C23(H23A,H23B,H23C)
4.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C17(H17), C19(H19), C14(H14), C18(H18), C10(H10), C3(H3), C20(H20),
 C9(H9), C13(H13), C11(H11)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C2(H2A,H2B,H2C)
4.e Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              59030
_olex2_submission_special_instructions 'No special instructions were received'