Antimony ??-diketonates and alkoxide/??-diketonates: remarkable formation of a 3,4-dihydro-2H-pyran ring by coupling of 1,1,1,5,5,5-hexafluoro-2,4-pentanedione ligands
Horley, Graeme A.; Mahon, Mary F.; Mazhar, Muhammed; Molloy, Kieran C.; Haycock, Peter W.; Myers, Christopher P.; Journal of the Chemical Society, Dalton Transactions  (2002) 4416–; doi:10.1039/b208110e

data_7012158
_publ_section_title
;
 Antimony ??-diketonates and alkoxide/??-diketonates: remarkable
 formation of a 3,4-dihydro-2H-pyran ring by coupling of
 1,1,1,5,5,5-hexafluoro-2,4-pentanedione ligands
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4416
_journal_paper_doi               10.1039/b208110e
_journal_year                    2002
_chemical_formula_sum            'C24 H43 O5 Sb'
_chemical_formula_weight         533.33
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.5830(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.4980(5)
_cell_length_b                   11.7800(2)
_cell_length_c                   18.3430(3)
_cell_measurement_temperature    170(2)
_cell_volume                     5458.20(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41874
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         4.66
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  0.7813
_exptl_absorpt_correction_T_min  0.6815
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.00025(14)
_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   0.755
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         7957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.755
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0982P)^2^+17.9881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                6143
_reflns_number_total             7957
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208110e.txt
_cod_data_source_block           k00kcm6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5458.20(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7012158