Towards clustered carbonyl cations [M3(CO)14]2+ (M = Ru, Os): the need for innocent deelectronation
Sellin, Malte; Friedmann, Christian; Mayländer, Maximilian; Richert, Sabine; Krossing, Ingo; Chemical Science 13 (2022) 9147–9158; doi:10.1039/D2SC02358J

data_1567450
_publ_section_title
;
 Towards clustered carbonyl cations [M3(CO)14]2+ (M = Ru, Os): the need
 for innocent deelectronation
;
_journal_issue                   32
_journal_name_full               'Chemical Science'
_journal_page_first              9147
_journal_page_last               9158
_journal_paper_doi               10.1039/D2SC02358J
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         '2(C16 Al F36 O4), C14 O14 Os3, 2(C6 H2 F4)'
_chemical_formula_sum            'C2.76 H0.19 Al0.1 F3.81 O1.05 Os0.14'
_chemical_formula_weight         152.25
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
FinalCif V98 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2022-02-08 deposited with the CCDC.	2022-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                71.674(9)
_cell_angle_beta                 71.730(7)
_cell_angle_gamma                73.486(9)
_cell_formula_units_Z            21
_cell_length_a                   11.283(3)
_cell_length_b                   14.143(3)
_cell_length_c                   15.714(3)
_cell_measurement_reflns_used    3311
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4575
_cell_measurement_theta_min      2.666
_cell_volume                     2211.9(9)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection       'Bruker BIS V6.2.14 Patch 4/2020-11-09'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13532
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.650
_diffrn_reflns_theta_min         1.408
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.556
_exptl_absorpt_correction_T_max  0.74607
_exptl_absorpt_correction_T_min  0.558513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1: Krause, L.,
Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.400
_exptl_crystal_description       block
_exptl_crystal_F_000             1502
_exptl_crystal_recrystallization_method
'diffusion of n-pentane in 1,2,3,4-tetrafluorobenzene'
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.193
_refine_diff_density_min         -2.394
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         13532
_refine_ls_number_restraints     3053
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0411
_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^)+16.6006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10982
_reflns_number_total             13532
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
'The data was integrated as a 2-component twin.'
_twin_individual_id              2
_twin_individual_twin_matrix_11  6e-05
_twin_individual_twin_matrix_12  0.00047
_twin_individual_twin_matrix_13  -1.00023
_twin_individual_twin_matrix_21  0.99952
_twin_individual_twin_matrix_22  -0.45124
_twin_individual_twin_matrix_23  -0.51557
_twin_individual_twin_matrix_31  -0.00218
_twin_individual_twin_matrix_32  -0.9993
_twin_individual_twin_matrix_33  -0.00038
_cod_data_source_file            d2sc02358j2.cif
_cod_data_source_block           p-1_a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1567449--1567458.cif.'
_cod_original_cell_volume        2211.8(8)
_cod_original_formula_sum        'C2.76 H0.19 Al0.10 F3.81 O1.05 Os0.14'
_cod_database_code               1567450
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.393
_shelx_estimated_absorpt_t_max   0.879
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_shelx_res_checksum              74220
_shelx_hkl_checksum              45007