Cyclometallated iridium complexes inducing paraptotic cell death like natural products: synthesis, structure and mechanistic aspects.
Tripathy, Suman Kumar; De, Umasankar; Dehury, Niranjan; Laha, Paltan; Panda, Manas Kumar; Kim, Hyung Sik; Patra, Srikanta; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15122–15136; doi:10.1039/c6dt00929h

data_7040352
_publ_section_title
;
 Cyclometallated iridium complexes inducing paraptotic cell death like
 natural products: synthesis, structure and mechanistic aspects.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15122
_journal_page_last               15136
_journal_paper_doi               10.1039/c6dt00929h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '2(C46 H32 Ir N6 S2), 2(F6 P), 3(C7 H8)'
_chemical_formula_sum            'C113 H88 F12 Ir2 N12 P2 S4'
_chemical_formula_weight         2416.53
_chemical_name_common            ThenilmIrPPy_LN_sq
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-04-14
_audit_creation_method
;

;
_audit_update_record
;
2016-07-27 deposited with the CCDC.
2016-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   49.358(8)
_cell_length_b                   49.358(8)
_cell_length_c                   11.9179(19)
_cell_measurement_reflns_used    9720
_cell_measurement_temperature    77(2)
_cell_measurement_theta_max      23.21
_cell_measurement_theta_min      2.18
_cell_volume                     25145(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      77.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.939
_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  0.1045
_diffrn_reflns_av_unetI/netI     0.0933
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       65
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_k_max       65
_diffrn_reflns_limit_k_min       -64
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            184536
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.283
_diffrn_reflns_theta_min         2.123
_exptl_absorpt_coefficient_mu    2.554
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       block
_exptl_crystal_F_000             10854
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.322
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         13028
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+385.7625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8934
_reflns_number_total             13028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00929h2.cif
_cod_data_source_block           mo_ThenilmIrPPy_LN_sq
_cod_depositor_comments
;Adding full bibliography for 7040351--7040352.cif.

 Adding full bibliography for 7040351--7040352.cif.
;
_cod_original_cell_volume        25145(9)
_cod_database_code               7040352
_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
2. Restrained distances
 C60-C55 = C56-C57 = C58-C59
 1.36 with sigma of 0.02
 C54-C60
 2.399 with sigma of 0.04
 C54-C56
 2.4 with sigma of 0.04
3. Restrained planarity
 C60, C59, C58, C57, C56, C55, C54
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C47 \\sim C48 \\sim C53 \\sim C52 \\sim C51 \\sim C50 \\sim C49: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C59 \\sim C60 \\sim C55 \\sim C56 \\sim C57 \\sim C58: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C54 \\sim C55: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C47) = Uanis(C48)
Uanis(C60) = Uanis(C59) = Uanis(C58) = Uanis(C57) = Uanis(C56) = Uanis(C55)
Uanis(C54) = Uanis(C55)
Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(S1)
5. Rigid body (RIGU) restrains
 C56, C55, C60, C59, C58, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C60(0.5) H60(0.5) C59(0.5) H59(0.5) C58(0.5) H58(0.5) C57(0.5)
 H57(0.5) C56(0.5) H56(0.5) C55(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5)
7.a Me refined with riding coordinates:
 C54(H54A,H54B,H54C)
7.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C1(H1), C35(H35), C23(H23), C26(H26), C41(H41), C2(H2), C30(H30),
 C29(H29), C32(H32), C37(H37), C36(H36), C44(H44), C42(H42), C9(H9), C10(H10),
 C15(H15), C25(H25), C8(H8), C3(H3), C16(H16), C17(H17), C24(H24), C20(H20),
 C21(H21), C49(H49), C51(H51), C22(H22), C50(H50), C52(H52), C53(H53), C60(H60),
  C59(H59), C58(H58), C57(H57), C56(H56)
7.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C34(H34A,H34B,H34C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              64347
_shelx_fab_checksum              22572
_olex2_submission_special_instructions 'No special instructions were received'