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_7708804
_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 Os P2,0.76 C H Cl3'
_chemical_formula_sum            'C37.77 H43.77 B9 Cl2.3 O Os P2'
_chemical_formula_weight         944.85
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-10-22 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                84.5650(17)
_cell_angle_beta                 78.068(2)
_cell_angle_gamma                71.413(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9431(3)
_cell_length_b                   12.4326(3)
_cell_length_c                   15.0763(3)
_cell_measurement_reflns_used    24096
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.82
_cell_measurement_theta_min      3.70
_cell_volume                     2074.98(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL and local programs'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SheLXT-2018/2
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Oxford Diffraction Gemini A Ultra diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            57342
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.905
_diffrn_reflns_theta_max         66.905
_diffrn_reflns_theta_min         3.975
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.119
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
   model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       prism
_exptl_crystal_F_000             937
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.768
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.080
_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     613
_refine_ls_number_reflns         7334
_refine_ls_number_restraints     363
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+3.0204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6700
_reflns_number_total             7334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02971a2.cif
_cod_data_source_block           ewc190009
_cod_original_formula_sum        'C37.77 H43.77 B9 Cl2.30 O Os P2'
_cod_database_code               7708804
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.323
_shelx_estimated_absorpt_t_max   0.737
_shelx_res_checksum              91037
_shelx_hkl_checksum              37043