Experimental and theoretical studies of pH-responsive iridium(III) complexes of azole and N-heterocyclic carbene ligands.
Hashemzadeh, Tahmineh; Christofferson, Andrew J.; White, Keith F.; Barnard, Peter J.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8478–8493; doi:10.1039/d3dt03766e

data_7715880
_publ_section_title
;
 Experimental and theoretical studies of pH-responsive iridium(III)
 complexes of azole and N-heterocyclic carbene ligands.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8478
_journal_page_last               8493
_journal_paper_doi               10.1039/d3dt03766e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C34 H25 Ir N5, Cl, 2(H2 O)'
_chemical_formula_sum            'C34 H29 Cl Ir N5 O2'
_chemical_formula_weight         767.27
_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             2024-03-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-08 deposited with the CCDC.	2024-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 132.839(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2393(2)
_cell_length_b                   28.2368(3)
_cell_length_c                   16.1627(4)
_cell_measurement_reflns_used    23663
_cell_measurement_temperature    159(40)
_cell_measurement_theta_max      69.5800
_cell_measurement_theta_min      3.7380
_cell_volume                     3091.9(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      160(40)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  SuperNova
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30792
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.239
_diffrn_reflns_theta_min         4.045
_exptl_absorpt_coefficient_mu    9.468
_exptl_absorpt_correction_T_max  0.93145
_exptl_absorpt_correction_T_min  0.93145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.396
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+11.8705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5770
_reflns_number_total             5812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03766e2.cif
_cod_data_source_block           13
_cod_depositor_comments
'Adding full bibliography for 7715878--7715882.cif.'
_cod_original_cell_volume        3091.93(18)
_cod_database_code               7715880
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.518
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O3(H3A,H3B)
2.b Free rotating group:
 O1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 N5(H5), C17(H17), C11(H11), C24(H24), C34(H34), C14(H14), C6(H6), C7(H7),
 C16(H16), C15(H15), C12(H12), C9(H9), C25(H25), C22(H22), C35(H35), C33(H33),
 C27(H27), C5(H5A), C19(H19), C21(H21), C10(H10), C26(H26), C20(H20), C32(H32),
 C31(H31)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 48 electrons were 
found in a volume of 140\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 1[H2O] per Formula Unit 
which account for 40 electrons per unit cell.
;
_shelx_res_checksum              35738
_shelx_fab_checksum              97858
_olex2_submission_special_instructions 'No special instructions were received'