Cyclometalated Ir(III) Complex as a Metalloligand and a Selective Cu(II) Sensor: Synthesis and Structural Characterization of a Heterometallic Tetranuclear Ir(III)/Cu(II) Complex.
Chandrasekhar, Vadapalli; Mahanti, Bani; Pandey, Mrituanjay D.; Narayanan, R. Suriya; ACS omega 3 (2018) 2786–2792; doi:10.1021/acsomega.8b00042

data_4516186
_publ_section_title
;
 Cyclometalated Ir(III) Complex as a Metalloligand and a Selective Cu(II)
 Sensor: Synthesis and Structural Characterization of a Heterometallic
 Tetranuclear Ir(III)/Cu(II) Complex.
;
_journal_issue                   3
_journal_name_full               'ACS omega'
_journal_page_first              2786
_journal_page_last               2792
_journal_paper_doi               10.1021/acsomega.8b00042
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C40 H29 Ir N6 O2'
_chemical_formula_sum            'C40 H29 Ir N6 O2'
_chemical_formula_weight         817.89
_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   geom
_audit_creation_date             2016-08-02
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.87(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.305(3)
_cell_length_b                   21.832(4)
_cell_length_c                   12.476(3)
_cell_measurement_reflns_used    1551
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.24
_cell_volume                     3546.5(14)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1447
_diffrn_reflns_av_unetI/netI     0.1757
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23478
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.911
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.808
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.513276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0674 before and 0.0466 after correction. The Ratio of minimum to maximum transmission is 0.5133. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.456
_refine_diff_density_min         -1.590
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6574
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1407
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3627
_reflns_number_total             6574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b00042_si_002.cif
_cod_data_source_block           1497274
_cod_original_cell_volume        3546.6(13)
_cod_database_code               4516186
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.618
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 N5(H5), C2(H2), C3(H3), C4(H4), C5(H5A), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C30(H30), C31(H31), C32(H32),
 C33(H33), C37(H37), C38(H38), C39(H39), C40(H40)
;
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'