Reversible Addition of Water to the High-Hydride-Content Cluster [Rh6(PiPr3)6H12][BArF4]2. Synthesis and Structure of [Rh6(PiPr3)6H11(OH)][BArF4]2
Thomas M. Douglas; Simon K. Brayshaw; Paul R. Raithby; Andrew S. Weller; Inorganic Chemistry 47 (2008) 778–780; doi:10.1021/ic702195b

data_4304654
_publ_section_title
;
Reversible Addition of Water to the High-Hydride-Content Cluster
[Rh6(PiPr3)6H12][BArF4]2. Synthesis and Structure of
[Rh6(PiPr3)6H11(OH)][BArF4]2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              778
_journal_page_last               780
_journal_paper_doi               10.1021/ic702195b
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C124 H154 B2 F50 O P6 Rh6'
_chemical_formula_weight         3435.37
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.340(1)
_cell_angle_beta                 68.189(1)
_cell_angle_gamma                88.444(1)
_cell_formula_units_Z            1
_cell_length_a                   13.3270(2)
_cell_length_b                   17.4040(2)
_cell_length_c                   17.8290(2)
_cell_measurement_reflns_used    68280
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.07
_cell_measurement_theta_min      3.73
_cell_volume                     3663.45(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
;
        "Collect" data collection software, Nonius' B.V., 1998.
;
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Nonius Kappa CCD'
_diffrn_measurement_method       'omega & phi scans'
_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  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            68280
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         3.73
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.7213
_exptl_absorpt_correction_T_min  0.6187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1726
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.189
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         21290
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+4.3189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                14290
_reflns_number_total             21290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702195b-file004.cif
_cod_data_source_block           k16asw23
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3663.45(8)
_cod_database_code               4304654