Reversible Ethylene Dihydrogen Mediated 11-Vertex nido\ρightarrowcloso\ρightarrownido Conversion in a Metallathiaborane Cluster
Álvaro Álvarez; Ramón Macías; María José Fabra; Fernando J. Lahoz; Luis A. Oro; Journal of the American Chemical Society 130 (2008) 2148–2149; doi:10.1021/ja078197j

data_4107443
_publ_contact_author_address
;
  Dr. Fernando J. Lahoz
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       lahoz@unizar.es
_publ_contact_author_fax         '+34 976 761187'
_publ_contact_author_name        'Dr. Fernando J. Lahoz'
_publ_contact_author_phone       '+34 976 761147'
_publ_section_title
;
 Reversible Ethylene Dihydrogen Mediated 11-Vertex
 nido\\rightarrowcloso\\rightarrownido Conversion in a Metallathiaborane
 Cluster
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2148
_journal_page_last               2149
_journal_paper_doi               10.1021/ja078197j
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C41 H45 B9 N P2 Rh S, C H Cl3, C Cl3'
_chemical_formula_sum            'C43 H46 B9 Cl6 N P2 Rh S'
_chemical_formula_weight         1083.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.481(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.922(3)
_cell_length_b                   15.436(3)
_cell_length_c                   12.930(3)
_cell_measurement_reflns_used    2340
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.825
_cell_measurement_theta_min      2.357
_cell_volume                     2431.4(9)
_computing_cell_refinement       'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w 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  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15295
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.9469
_exptl_absorpt_correction_T_min  0.8795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.45.                    
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1098
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.953
_refine_diff_density_min         -1.729
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.15(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         7878
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+2.3957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                6575
_reflns_number_total             7878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja078197j-file002.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        2431.7(8)
_cod_database_code               4107443