Synthesis of Novel Molybdaboranes from (η5-C5R5)MoCln Precursors (R = H, Me; n= 1, 2, 4)
Simon Aldridge; Maoyu Shang; Thomas P. Fehlner; Journal of the American Chemical Society 120 (1998) 2586–2598; doi:10.1021/ja973720n

data_4116705
_publ_section_title
;
 Synthesis of Novel Molybdaboranes from (\h5-C5R5)MoCln Precursors (R = H,
 Me; n= 1, 2, 4)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2586
_journal_page_last               2598
_journal_paper_doi               10.1021/ja973720n
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C20 H35.19 B1.73 Cl2.27 Mo2'
_chemical_formula_weight         566.73
_chemical_name_systematic
; 
 (Me5CpMo)2Cl2(B2H6)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 108.61(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1278(7)
_cell_length_b                   29.447(6)
_cell_length_c                   10.601(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2404.6(11)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johoson, 1996)'
_computing_publication_material  'SHELXTL-V5 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius FAST area-detector'
_diffrn_measurement_method       'ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9999
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7947
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       wedge-like
_exptl_crystal_F_000             1146
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.094
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_hydrogen_treatment
;
idealized riding model for Cp rings, bond length restraints by a model of
an idealized tetrahedral borane geometry.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         6342
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.117
_refine_ls_restrained_S_obs      1.071
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_obs          0.0683
_refine_ls_shift/esd_max         -0.135
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+21.8347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1745
_refine_ls_wR_factor_obs         0.1466
_reflns_number_observed          4952
_reflns_number_total             6360
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja973720n.cif
_cod_data_source_block           JA973720N-275
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+21.8347P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+21.8347P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2404.6(10)
_cod_database_code               4116705