Synthesis, structural characterization and biological properties of cyclometalated iridium(iii) complexes containing [1,2,5]-thiadiazolo-[3,4-f]-[1,10]-phenanthroline
Bhat, Satish S.; S., Naveen; Revankar, Vidyanand K.; Lokanath, N. K.; Pinjari, Rahul V.; Kumbar, Vijay; Bhat, Kishore; New Journal of Chemistry 44 (2020) 17442–17452; doi:10.1039/D0NJ03421E

data_7059990
_publ_section_title
;
 Synthesis, structural characterization and biological properties of
 cyclometalated iridium(iii) complexes containing
 [1,2,5]-thiadiazolo-[3,4-f]-[1,10]-phenanthroline
;
_journal_issue                   40
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17442
_journal_page_last               17452
_journal_paper_doi               10.1039/D0NJ03421E
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety
'C34 H22 Ir N6 S, Cl, C H4 O, 3(H2 O)'
_chemical_formula_sum            'C35 H32 Cl Ir N6 O4 S'
_chemical_formula_weight         860.37
_chemical_properties_physical    Air-sensitive,Light-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-02-03 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.4560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.4273(5)
_cell_length_b                   13.5792(4)
_cell_length_c                   27.8866(8)
_cell_measurement_temperature    296(2)
_cell_volume                     6527.6(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            45891
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        64.505
_diffrn_reflns_theta_max         64.505
_diffrn_reflns_theta_min         2.563
_exptl_absorpt_coefficient_mu    9.686
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_F_000             3404
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Vapour deposition'
_refine_diff_density_max         1.831
_refine_diff_density_min         -1.595
_refine_diff_density_rms         0.377
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         10720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0499
_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^)+(0.1071P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9725
_reflns_number_total             10720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03421e2.cif
_cod_data_source_block           ir2bs
_cod_depositor_comments
;
Adding full bibliography for 7059990--7059991.cif.

2024-11-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C70 H63 Cl2 Ir2 N12 O8 S2'
_cod_original_formula_weight         1719.74
_cod_original_formula_moiety
'2(C34 H22 Ir N6 S), 2(Cl), 2(C H4 O), 5(H2 O), H O'
_cod_original_formula_units_Z            4
_cod_database_code               7059990
_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, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O6(H6A,H6B), O9(H9A,H9B), O1AA(H1AD,H1AE), O0AA(H0AD,H0AE), O2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C13(H13), C00K(H00K), C20(H20), C00R(H00R), C010(H010),
 C011(H011), C013(H013), C16(H16), C10(H10), C21(H21), C01C(H01C), C01D(H01D),
 C01F(H01F), C01H(H01H), C01I(H01I), C01K(H01K), C33(H33), C22(H22), C1(H1),
 C24(H24), C8(H8), C01T(H01T), C01V(H01V), C9(H9), C14(H14), C01Y(H01Y),
 C01Z(H01Z), C23(H23), C021(H021), C25(H25), C27(H27), C15(H15), C027(H027),
 C028(H028), C26(H26), C02A(H02A), C3(H3), C02F(H02F), C02G(H02G), C2(H2),
 C32(H32), C31(H31), C30(H30)
2.c Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC)
2.d Idealised tetrahedral OH refined as rotating group:
 O5(H5), O7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'