Preparation and properties of sterically demanding and chiral distibine ligands
Jura, Marek; Levason, William; Reid, Gillian; Webster, Michael; Dalton Transactions  (2008) 5774–5782; doi:10.1039/b808493a

data_7004554
_publ_section_title
;
 Preparation and properties of sterically demanding and chiral
 distibine ligands
;
_journal_issue                   42
_journal_name_full               'Dalton Transactions'
_journal_page_first              5774
_journal_page_last               5782
_journal_paper_doi               10.1039/b808493a
_journal_year                    2008
_chemical_formula_moiety         'C28 H36 O4 Sb4'
_chemical_formula_structural     '(C14 H18 Sb2)2 O4'
_chemical_formula_sum            'C28 H36 O4 Sb4'
_chemical_formula_weight         923.57
_chemical_name_common
bis((1,8-bis(dimethylstibino)naphthalene)di(mu!3$-oxido))
_chemical_name_systematic
;
bis((1,8-bis(dimethylstibino)naphthalene)di(\m~3~-oxido))
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-06-20
_audit_creation_method           'SHELXL-97 + hand edit'
_audit_update_record
' 2008-06-20 revised (improved) disorder treatment of 1 naphthyl group.'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.032(2)
_cell_length_b                   13.1268(10)
_cell_length_c                   10.7375(10)
_cell_measurement_reflns_used    3592
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2823.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23985
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.819
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.875
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.376
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3358
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.375
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+26.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                3114
_reflns_number_total             3358
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b808493a.txt
_cod_data_source_block           07mj004_[C28H36O4Sb4]
_cod_database_code               7004554