A simple and high-yield route to iridium, rhodium, osmium and ruthenium nido-6-metalladecaborane compounds
Bould, Jonathan; Londesborough, Michael G. S.; Passarelli, Vincenzo; Clegg, William; Waddell, Paul G.; Cvačka, Josef; Macías, Ramón; Dalton Transactions  (2021) –; doi:10.1039/D1DT02971A

data_7708801
_publ_section_title
;
 A simple and high-yield route to iridium, rhodium, osmium and ruthenium
 nido-6-metalladecaborane compounds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02971A
_journal_year                    2021
_chemical_formula_moiety         'C37 H43 B9 O P2 Ru'
_chemical_formula_sum            'C37 H43 B9 O P2 Ru'
_chemical_formula_weight         764.01
_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   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-07-16 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                89.307(7)
_cell_angle_beta                 88.185(4)
_cell_angle_gamma                89.273(5)
_cell_formula_units_Z            4
_cell_length_a                   10.562(3)
_cell_length_b                   15.544(5)
_cell_length_c                   22.521(8)
_cell_measurement_reflns_used    9713
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.297
_cell_measurement_theta_min      2.604
_cell_volume                     3695(2)
_computing_cell_refinement       'SAINT+ in APEX2 (Bruker AXS,2008)'
_computing_data_collection       'SMART in APEX2 (Bruker AXS,2008)'
_computing_data_reduction        'SAINT+ in APEX2 (Bruker AXS,2008)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX DUO system'
_diffrn_measurement_method       '\w and \f rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            98919
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.382
_diffrn_reflns_theta_min         1.310
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  0.8496
_exptl_absorpt_correction_T_min  0.6634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008), TWINABS, University of Gottingen
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       prism
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         18360
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+6.5298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15215
_reflns_number_total             18360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02971a2.cif
_cod_data_source_block           compound_3_VPX162D_JB145
_cod_database_code               7708801
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              73787
_shelx_hkl_checksum              12269