Methylation of Ir( <scp>iii</scp> )-tetrazolato complexes: an effective route to modulate the emission outputs and to switch to antimicrobial properties
Fiorini, Valentina; Zanoni, Ilaria; Zacchini, Stefano; Costa, Anna Luisa; Hochkoeppler, Alejandro; Zanotti, Valerio; Ranieri, Anna Maria; Massi, Massimiliano; Stefan, Alessandra; Stagni, Stefano; Dalton Transactions 46 (2017) 12328–12338; doi:10.1039/C7DT02352A

data_1546853
_publ_section_title
;
 Methylation of Ir( <scp>iii</scp> )-tetrazolato complexes: an effective
 route to modulate the emission outputs and to switch to antimicrobial
 properties
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              12328
_journal_page_last               12338
_journal_paper_doi               10.1039/C7DT02352A
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C33 H25 F6 Ir N7 P'
_chemical_formula_weight         856.77
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-27 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.604(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.4719(5)
_cell_length_b                   18.6483(10)
_cell_length_c                   41.050(2)
_cell_measurement_reflns_used    5017
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.432
_cell_measurement_theta_min      2.240
_cell_volume                     6472.5(6)
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3090
_diffrn_reflns_av_unetI/netI     0.1973
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            61336
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        23.531
_diffrn_reflns_theta_max         23.531
_diffrn_reflns_theta_min         1.477
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.246
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5615
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1441 (selected reflections only, before parameter refinement)
 R(int) =  0.0922 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_description       needle
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.291
_refine_diff_density_min         -2.043
_refine_diff_density_rms         0.227
_refine_ls_extinction_coef       0.00036(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         9620
_refine_ls_number_restraints     1008
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1711
_refine_ls_R_factor_gt           0.0817
_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^)+(0.0413P)^2^+101.2475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5260
_reflns_number_total             9620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02352a2.cif
_cod_data_source_block           IrQTZMe
_cod_depositor_comments
;

2019-01-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C66 H50 F12 Ir2 N14 P2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1713.54
_cod_database_code               1546853
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.588
_shelx_estimated_absorpt_t_max   0.755
_shelx_res_checksum              74206
_shelx_fab_checksum              17087