Bis-cyclometallated Ir(III) complexes containing 2-(1<i>H</i>-pyrazol-3-yl)pyridine ligands; influence of substituents and cyclometallating ligands on response to changes in pH.
Abdolla, Noreldin S. Y.; Davies, David L.; Lowe, Mark P.; Singh, Kuldip; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12025–12036; doi:10.1039/d0dt02434a

data_7705151
_publ_section_title
;
 Bis-cyclometallated Ir(III) complexes containing
 2-(1<i>H</i>-pyrazol-3-yl)pyridine ligands; influence of substituents and
 cyclometallating ligands on response to changes in pH.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12025
_journal_page_last               12036
_journal_paper_doi               10.1039/d0dt02434a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C34 H31 Ir N5, F6 P, 0.5(H2 O), C6 H14'
_chemical_formula_sum            'C40 H46 F6 Ir N5 O0.5 P'
_chemical_formula_weight         941.99
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2020-07-07 deposited with the CCDC.	2020-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                91.865(7)
_cell_angle_beta                 100.706(7)
_cell_angle_gamma                93.332(7)
_cell_formula_units_Z            4
_cell_length_a                   11.648(5)
_cell_length_b                   16.487(7)
_cell_length_c                   19.704(9)
_cell_measurement_reflns_used    1002
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.141
_cell_measurement_theta_min      2.396
_cell_volume                     3708(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_sigmaI/netI    0.1234
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28454
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    3.713
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.397
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 11055 reflections(SADABS);Rint 0.1662 before
correction and 0.0562 after.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;

Disordered C6H14 was omitted using the SQUEEZE option of PLATON. The solvent
accessible voids are 641.3 ?3 with an estimated 221e/cell to be added. Four 
solvent C6H14 molecules/unit cell accounting for 200e were included in the 
formula, FWt, (000) and density calculations. PLATON Reference:
Spek, A.L. (1990), Acta Cryst. A46, C-34.  

;
_refine_diff_density_max         3.715
_refine_diff_density_min         -1.839
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         14329
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                9143
_reflns_number_total             14329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt02434a2.cif
_cod_data_source_block           15068
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7705149--7705156.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C80 H92 F12 Ir2 N10 O P2'
_cod_original_formula_weight         1883.98
_cod_original_formula_moiety         '2(C34 H31 Ir N5), 2(F6 P), H2 O,2 C6 H14'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7705151