Crystal structure of 1-[3-(trifluoromethyl)cinnamoyl]-3-(pyridin-2-yl-κN)pyrazole-κ2 N-bis(2-phenylpyridinato-k2 C,N)iridium(III) hexafluorophosphate complex, [C40H28F3IrN5O]PF6
Chong, Yan Yi; Mark-Lee, Wun Fui; Ahmad, Ishak; Kassim, Mohammad B.; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 825–829; doi:10.1515/ncrs-2020-0029

data_8105299
_publ_section_title
;
 Crystal structure of
 1-[3-(trifluoromethyl)cinnamoyl]-3-(pyridin-2-yl-\kN)pyrazole-\k2
 N-bis(2-phenylpyridinato-k2 C,N)iridium(III) hexafluorophosphate complex,
 [C40H28F3IrN5O]PF6
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              825
_journal_page_last               829
_journal_paper_doi               10.1515/ncrs-2020-0029
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C40 H28 F3 Ir N5 O,F6 P'
_chemical_formula_sum            'C40 H28 F9 Ir N5 O P'
_chemical_formula_weight         988.86
_chemical_name_systematic
;
1-[3-(trifluoromethyl)cinnamoyl]-3-(pyridin-2-yl-<i>kN</i>)pyrazole-
<i>kN^2^</i>-bis(2-phenylpyridinato-<i>k^2^C,N</i>)iridium(III)
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 96.937(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2282(19)
_cell_length_b                   14.5095(11)
_cell_length_c                   12.6091(10)
_cell_measurement_reflns_used    9234
_cell_measurement_temperature    107
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      3.0
_cell_volume                     3673.7(5)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_molecular_graphics    'OLEX2(Dolomanov et al., 2009)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), PLATON (Spek, 2009), OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015), shelXle(H\"ubschle et. al, 2011)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      107(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1821
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            112848
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.338
_diffrn_reflns_theta_min         2.985
_diffrn_source                   'Incoatec Microfocus'
_exptl_absorpt_coefficient_mu    3.765
_exptl_absorpt_correction_T_max  0.6768
_exptl_absorpt_correction_T_min  0.4327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.880
_refine_diff_density_min         -2.064
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details
;
 Flack x determined using 2218 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9126
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      16.352
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+17.7470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6926
_reflns_number_total             9126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0029_suppl.cif
_cod_data_source_block           b_17052018
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_colour_primary' value 'Orange' was changed
to 'orange' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               8105299
_shelx_estimated_absorpt_t_max   0.682
_shelx_estimated_absorpt_t_min   0.398