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_7012156
_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            'C33 H57 O6 Sb'
_chemical_formula_weight         671.54
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                77.86(2)
_cell_angle_beta                 69.81(2)
_cell_angle_gamma                78.49(2)
_cell_formula_units_Z            2
_cell_length_a                   10.146(3)
_cell_length_b                   13.272(3)
_cell_length_c                   14.361(4)
_cell_measurement_temperature    170(2)
_cell_volume                     1757.3(9)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0142
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6677
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  1.030
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   'semi-empirical from equivalents'
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.656
_refine_ls_goodness_of_fit_obs   0.647
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.675
_refine_ls_restrained_S_obs      0.647
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_obs          0.0315
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1532P)^2^+4.3998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1261
_refine_ls_wR_factor_obs         0.1124
_reflns_number_observed          5363
_reflns_number_total             6166
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b208110e.txt
_cod_data_source_block           99kcm14
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1532P)^2^+4.3998P] 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^)+(0.1532P)^2^+4.3998P] 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        1757.3(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012156