Metallaheteroborane chemistry: Part 16.Part 15: ref. 1. Contrasting metal to heteroborane bonding modes in isoelectronic {MC2B9} and {MAs2B9} clusters. Synthesis and characterisation of [9-{Fe(CO)2(?5-C5H5)}-nido-7,8-C2B9H12], [7-{Fe(CO)2(?5-C5H5)}-nido-7,8-As2B9H10] and [7-{M(CO)2(?7-C7H7)}-nido-7,8-As2B9H10], where M is Mo or W
Bould, Jonathan; Kennedy, John D.; Ferguson, George; Tony Deeney, F.; O'Riordan, Gerald M.; Spalding, Trevor R.; Dalton Transactions  (2003) 4557–; doi:10.1039/b306776a

data_7013364
_publ_section_title
;
 Metallaheteroborane chemistry: Part 16.Part 15: ref. 1. Contrasting
 metal to heteroborane bonding modes in isoelectronic {MC2B9} and
 {MAs2B9} clusters. Synthesis and characterisation of
 [9-{Fe(CO)2(?5-C5H5)}-nido-7,8-C2B9H12],
 [7-{Fe(CO)2(?5-C5H5)}-nido-7,8-As2B9H10] and
 [7-{M(CO)2(?7-C7H7)}-nido-7,8-As2B9H10], where M is Mo or W
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              4557
_journal_paper_doi               10.1039/b306776a
_journal_year                    2003
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesized by the authors, see text'
_chemical_formula_moiety         'C9 H17 As2 B9 Mo O2'
_chemical_formula_sum            'C9 H17 As2 B9 Mo O2'
_chemical_formula_weight         500.30
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6069(14)
_cell_length_b                   10.8092(14)
_cell_length_c                   14.188(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(1)
_cell_measurement_theta_max      20.14
_cell_measurement_theta_min      9.56
_cell_volume                     1780.0(4)
_computing_cell_refinement       'SET4 & CELDIM (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD4 (Enraf-Nonius, 1992)'
_computing_data_reduction        'DATRD2 in NRCVAX96 (Gabe et al., 1989)'
_computing_molecular_graphics
'NRCVAX96, ORTEP (Johnson, 1976), PLATON (Spek, 1998)'
_computing_publication_material
'NRCVAX96, SHELXL97  and WordPerfect macro PREP8 (Ferguson, 1998)'
_computing_structure_refinement  'NRCVAX96 and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'NRCVAX96 via Patterson heavy-atom method'
_diffrn_ambient_temperature      294(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4244
_diffrn_reflns_theta_full        26.90
_diffrn_reflns_theta_max         26.90
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.422
_exptl_absorpt_correction_T_max  0.2287
_exptl_absorpt_correction_T_min  0.1869
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          .412
_exptl_crystal_size_mid          .33
_exptl_crystal_size_min          .3325
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.881
_refine_ls_abs_structure_details 'Flack (1983), 1664 Friedel pairs'
_refine_ls_abs_structure_Flack   0.011(16)
_refine_ls_extinction_coef       0.0017(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3871
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0710P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                3191
_reflns_number_total             3871
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b306776a.txt
_cod_data_source_block           3
_cod_database_code               7013364