Heteroleptic [Os(Cl)(CO)(P^P)(pbi)] complexes bearing bidentate phosphine and 2-(2-pyridyl)benzimidazolate ligands: impact of isomerism on their luminescence properties
Kamecka, Anna; Suwińska, Kinga; Kapturkiewicz, Andrzej; Physical Chemistry Chemical Physics  (2019) –; doi:10.1039/C9CP03416A

data_7233313
_publ_section_title
;
 Heteroleptic [Os(Cl)(CO)(P^P)(pbi)] complexes bearing bidentate phosphine
 and 2-(2-pyridyl)benzimidazolate ligands: impact of isomerism on their
 luminescence properties
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/C9CP03416A
_journal_year                    2019
_chemical_formula_moiety         'C39 H32 Cl N3 O Os P2, 0.5(C3 H7 OH)'
_chemical_formula_sum            'C40.5 H36 Cl N3 O1.5 Os P2'
_chemical_formula_weight         876.31
_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_Hall           'I 4bw'
_space_group_name_H-M_alt        'I 41'
_symmetry_space_group_name_Hall  'I 4bw'
_symmetry_space_group_name_H-M   'I 41'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc22dhcc
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-07-17 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   23.138(3)
_cell_length_b                   23.138(3)
_cell_length_c                   26.906(3)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.253
_cell_measurement_theta_min      2.490
_cell_volume                     14405(3)
_computing_cell_refinement       'APEX3 v2015.9-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v4.2.9'
_computing_data_reduction        'SAINT V8.35A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'Mercury CSD 4.1.2 (2019)'
_computing_publication_material  'APEX3 v2015.9-0 (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'D8 VENTURE DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_unetI/netI     0.1523
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            66897
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.581
_diffrn_reflns_theta_min         1.960
_diffrn_source                   I\mS
_exptl_absorpt_coefficient_mu    3.743
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       needle
_exptl_crystal_F_000             6960
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.065
_refine_diff_density_max         1.444
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.212
_refine_ls_abs_structure_details
;
 Flack x determined using 4464 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.166(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         20025
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0172P)^2^+9.2369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.855
_reflns_number_gt                12873
_reflns_number_total             20025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cp03416a1.cif
_cod_data_source_block           Os_pbi_dppe2
_cod_original_cell_volume        14404(4)
_cod_original_formula_sum        'C40.50 H36 Cl N3 O1.50 Os P2'
_cod_database_code               7233313
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.402
_shelx_estimated_absorpt_t_max   0.793
_shelx_res_checksum              76336
_shelx_hkl_checksum              46726