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_7708803
_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_absolute_configuration ad
_chemical_formula_moiety         'C35 H46 B9 O P3 Pt Ru'
_chemical_formula_sum            'C35 H46 B9 O P3 Pt Ru'
_chemical_formula_weight         969.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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
;
2021-08-15 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.8368(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.49283(13)
_cell_length_b                   16.98921(13)
_cell_length_c                   11.52564(15)
_cell_measurement_reflns_used    19016
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.85
_cell_measurement_theta_min      4.26
_cell_volume                     2008.05(5)
_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
_computing_structure_solution    SHELXT-2018/2
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0256
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28920
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        66.913
_diffrn_reflns_theta_max         66.913
_diffrn_reflns_theta_min         4.299
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    10.796
_exptl_absorpt_correction_T_max  0.658
_exptl_absorpt_correction_T_min  0.252
_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    1.603
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane and hexane'
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 2891 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.042(4)
_refine_ls_extinction_coef       0.00005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         6668
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0151
_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^)+(0.0187P)^2^+0.1917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0338
_refine_ls_wR_factor_ref         0.0341
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.863
_reflns_Friedel_fraction_max     0.863
_reflns_number_gt                6589
_reflns_number_total             6668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02971a2.cif
_cod_data_source_block           ewc190013_compound6
_cod_original_cell_volume        2008.05(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7708803
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.210
_shelx_estimated_absorpt_t_max   0.672
_shelx_res_checksum              42051
_shelx_hkl_checksum              5944