Towards efficient Ir(III) anticancer photodynamic therapy agents by extending π-conjugation on N^N ligands.
Sanz-Villafruela, Juan; Bermejo-Casadesús, Cristina; Martínez-Alonso, Marta; Moro, Artur; Lima, João C; Massaguer, Anna; Espino, Gustavo; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11393–11409; doi:10.1039/d4dt00390j

data_7716389
_publ_section_title
;
 Towards efficient Ir(III) anticancer photodynamic therapy agents by
 extending &#x3c0;-conjugation on N^N ligands.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11393
_journal_page_last               11409
_journal_paper_doi               10.1039/d4dt00390j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C46 H30 Ir N6, Cl'
_chemical_formula_sum            'C46 H30 Cl Ir N6'
_chemical_formula_weight         894.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-01-23 deposited with the CCDC.	2024-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.143(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.101(2)
_cell_length_b                   21.839(2)
_cell_length_c                   17.1508(18)
_cell_measurement_reflns_used    9751
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.60
_cell_volume                     8426.0(14)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      301.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1115
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            132320
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.664
_diffrn_reflns_theta_min         2.439
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.270
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1447 before and 0.0944 after correction.
The Ratio of minimum to maximum transmission is 0.4812.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       prism
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.170
_refine_diff_density_min         -2.246
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0496P)^2^+87.4887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7071
_reflns_number_total             9754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00390j2.cif
_cod_data_source_block           1_a
_cod_depositor_comments          'Adding full bibliography for 7716389.cif.'
_cod_original_cell_volume        8426.0(15)
_cod_database_code               7716389
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.355
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N6(H6A), C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9),
 C10(H10), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C34(H34), C35(H35),
 C36(H36), C37(H37), C43(H43), C44(H44), C45(H45), C46(H46)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51740
_shelx_fab_checksum              49864
_olex2_submission_special_instructions 'No special instructions were received'