Yttrium β-diketonate complexes with triglyme: ionic and neutral isomers and outer-sphere co-ordination of triglyme †
Pollard, Kimberly D.; Vittal, Jagadese J.; Yap, Glenn P. A.; Puddephatt, Richard J.; Journal of the Chemical Society, Dalton Transactions  (1998) 1265–; doi:10.1039/a801344f

data_7028081
_publ_section_title
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 Yttrium \b-diketonate complexes with triglyme: ionic and neutral isomers
 and outer-sphere co-ordination of triglyme&#x200A;&#x2020;
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_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1265
_journal_paper_doi               10.1039/a801344f
_journal_year                    1998
_chemical_formula_sum            'C23 H25 F18 O12 Y'
_chemical_formula_weight         924.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   12.0579(2)
_cell_length_b                   12.0579(2)
_cell_length_c                   44.7674(9)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      1.47
_cell_volume                     5636.84(17)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL XPREP'
_computing_molecular_graphics    'Siemens SHELXTL XP'
_computing_publication_material  'Siemens SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       'hemisphere scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_av_sigmaI/netI    0.0642
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            31888
_diffrn_reflns_theta_max         20.99
_diffrn_reflns_theta_min         1.36
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    1.692
_exptl_absorpt_correction_T_max  0.801477
_exptl_absorpt_correction_T_min  0.456808
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       plate
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.120
_refine_ls_goodness_of_fit_obs   1.161
_refine_ls_hydrogen_treatment    idealized
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         4022
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.149
_refine_ls_restrained_S_obs      1.153
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_obs          0.0803
_refine_ls_shift/esd_max         -0.113
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0894P)^2^+7.9196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1871
_refine_ls_wR_factor_obs         0.1715
_reflns_number_observed          3393
_reflns_number_total             4032
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            f801344sup1.cif
_cod_data_source_block           rp013
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0894P)^2^+7.9196P] 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^)+(0.0894P)^2^+7.9196P] 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        5636.8(2)
_cod_original_sg_symbol_H-M      P3(1)21
_cod_database_code               7028081