Compounds containing λ3,σ2-SbC bonds: synthesis and structural characterisation of the first stiba-enol, Mes*C(O)SbC(OH)Mes* (Mes* = C6H2But3-2,4,6) and a 2,3-distibabutadiene, {Mes(Me3SiO)CSb}2 (Mes = C6H2Me3-2,4,6) †
Jones, Cameron; Steed, Jonathan W.; Thomas, Ryan C.; Journal of the Chemical Society, Dalton Transactions  (1999) 1541–; doi:10.1039/a902791b

data_7027441
_publ_section_title
;
 Compounds containing \l3,\s2-Sb&#xE006;C bonds: synthesis and structural
 characterisation of the first stiba-enol, Mes*C(O)Sb&#xE006;C(OH)Mes*
 (Mes*&#x2005;=&#x2005;C6H2But3-2,4,6) and a 2,3-distibabutadiene,
 {Mes(Me3SiO)C&#xE006;Sb}2
 (Mes&#x2005;=&#x2005;C6H2Me3-2,4,6)&#x200A;&#x2020;
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1541
_journal_paper_doi               10.1039/a902791b
_journal_year                    1999
_chemical_formula_sum            'C26 H40 O2 Sb2 Si2'
_chemical_formula_weight         684.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 109.57(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.704(2)
_cell_length_b                   14.043(3)
_cell_length_c                   10.889(2)
_cell_measurement_temperature    100(2)
_cell_volume                     1542.2(6)
_computing_cell_refinement       DENZOSMN
_computing_data_reduction        DENZOSMN
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '2o phi frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13007
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.848
_exptl_absorpt_correction_type   scalepack
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1.
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.0029(7)
_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   0.502
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.502
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1309P)^2^+26.8922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                2474
_reflns_number_total             3028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            902791bsup1.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1542.2(5)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7027441