Synthesis of [Os(bpy)2(py)(OH2)](PF6)x substituted pyridine complexes; characterization of a singly bridged H3O2− ligand
Sun, Jiangtian; Sun, Jingwen; Jolly, Brandon J.; Riu, Martin-Louis Y.; Kerr, Tyler A.; Lai, Yi-An; Pung, Michael J.; Liu, Chong; Nava, Matthew; Dalton Transactions 54 (2025) 5109–5118; doi:10.1039/D5DT00419E

data_7718102
_publ_section_title
;
 Synthesis of [Os(bpy)2(py)(OH2)](PF6)x substituted pyridine complexes;
 characterization of a singly bridged H3O2&#x2212; ligand
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              5109
_journal_page_last               5118
_journal_paper_doi               10.1039/D5DT00419E
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum
'C4.51 H5.43 Cl0.1 F1.23 N0.77 O0.41 Os0.15 P0.21'
_chemical_formula_weight         139.66
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;FinalCif V136 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-06-07 deposited with the CCDC.	2025-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.552(2)
_cell_angle_gamma                90
_cell_formula_units_Z            26
_cell_length_a                   17.1152(10)
_cell_length_b                   8.7658(5)
_cell_length_c                   22.3304(14)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0845
_cell_measurement_theta_min      2.873
_cell_volume                     3270.1(3)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection       'Bruker BIS V6.2.12/2019-08-12'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker Photon III Area Detector'
_diffrn_detector_area_resol_mean 7.407
_diffrn_detector_type            'CPAD Area Detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            63243
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.590
_diffrn_reflns_theta_min         2.731
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_current           50.0
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.104
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction: 
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 
(2015) 3-10
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_description       plate
_exptl_crystal_F_000             1788
_exptl_crystal_recrystallization_method 'Ethanol - Diethyl Ether Layering'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.315
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         9264
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+10.4464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7227
_reflns_number_total             9264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00419e2.cif
_cod_data_source_block           nava2409
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' 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 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7718102--7718103.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum
'C4.51 H5.43 Cl0.10 F1.23 N0.77 O0.41 Os0.15 P0.21'
_cod_database_code               7718102
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              3239