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_1567451
_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         'C16 Al F36 O4, C13 N O13 Ru4'
_chemical_formula_sum            'C29 Al F36 N O17 Ru4'
_chemical_formula_weight         1749.56
_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_primary     direct
_audit_creation_method
;
FinalCif V98 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2022-02-11 deposited with the CCDC.	2022-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.87(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.639(14)
_cell_length_b                   15.156(14)
_cell_length_c                   41.36(4)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.2605
_cell_measurement_theta_min      2.2595
_cell_volume                     9752(16)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection
'Bruker BIS 2018.9.0.3/05-Dec-2018 && APEX3_2019.1-0'
_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                 'Image Plate'
_diffrn_detector_type            'Rigaku Image Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1000
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            135688
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.022
_diffrn_reflns_theta_min         0.990
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.440
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5889
_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    2.383
_exptl_crystal_description       plate
_exptl_crystal_F_000             6640
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2,3,4-Tetrafluorobenzene, n-pentane'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.807
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1966
_refine_ls_number_reflns         23163
_refine_ls_number_restraints     19111
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0306P)^2^+3.5066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15319
_reflns_number_total             23163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02358j2.cif
_cod_data_source_block           p21c_a
_cod_depositor_comments
'Adding full bibliography for 1567449--1567458.cif.'
_cod_original_cell_volume        9752(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1567451
_shelx_shelxl_version_number     2018/3
_olex2_diffrn_ambient_temperature_device 'Bruker Kryoflex II'
_shelx_res_checksum              89383
_shelx_hkl_checksum              81175