10-Vertex Manganese−Dicarbollide Complexes from a Monocarbon Precursor. Synthesis and Cluster Vertex Functionalization of [1-OH-2,2,2-(CO)3-closo-2,1,10-MnC2B7H8]−
Franken, Andreas; McGrath, Thomas D.; Stone, F. Gordon A.; Organometallics 28 (2009) 225–; doi:10.1021/om800730n

data_4068343
_publ_section_title
;
 10-Vertex Manganese&#x2212;Dicarbollide Complexes from a Monocarbon
 Precursor. Synthesis and Cluster Vertex Functionalization of
 [1-OH-2,2,2-(CO)3-closo-2,1,10-MnC2B7H8]&#x2212;
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              225
_journal_paper_doi               10.1021/om800730n
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C41 H39 B7 Mn N O3 P2'
_chemical_formula_weight         786.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.6834(18)
_cell_length_b                   17.0989(15)
_cell_length_c                   11.0349(9)
_cell_measurement_reflns_used    3586
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.88
_cell_measurement_theta_min      2.59
_cell_volume                     3902.6(6)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2003)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2003)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2003)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 2001)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'Bruker SHELXTL (Bruker, 2001)'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker-Nonius X8 APEX CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0957
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35961
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.64
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  0.9693
_exptl_absorpt_correction_T_min  0.9345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7307
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0484P)^2^+1.9534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                5655
_reflns_number_total             7307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800730n_si_001.cif
_cod_data_source_block           15
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               4068343