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_7233314
_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, H2 O'
_chemical_formula_sum            'C39 H34 Cl N3 O2 Os P2'
_chemical_formula_weight         864.28
_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_block_doi                 10.5517/ccdc.csd.cc22dhbb
_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                 101.198(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.170(4)
_cell_length_b                   11.651(2)
_cell_length_c                   16.431(3)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0840
_cell_measurement_theta_min      2.3144
_cell_volume                     3412.2(11)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.3513
_diffrn_reflns_av_unetI/netI     0.1147
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            107932
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.777
_diffrn_reflns_theta_max         24.777
_diffrn_reflns_theta_min         2.088
_diffrn_source                   I\mS
_exptl_absorpt_coefficient_mu    3.950
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       needle
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.825
_refine_diff_density_min         -2.157
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       0.0029(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         5802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1211
_refine_ls_R_factor_gt           0.0731
_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^)+(0.0367P)^2^+60.9916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4019
_reflns_number_total             5802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cp03416a1.cif
_cod_data_source_block           Os_pbi_dppe1
_cod_original_cell_volume        3412.1(12)
_cod_database_code               7233314
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.350
_shelx_estimated_absorpt_t_max   0.868
_shelx_res_checksum              59150
_shelx_hkl_checksum              65157