Lanthanide(III) Methylsquarates: Synthesis and X-ray Structures
Bert D. Alleyne; Avril R. Williams; Lincoln A. Hall; Andrew J. P. White; David J. Williams; Inorganic Chemistry 40 (2001) 1045–1051; doi:10.1021/ic000989q

data_4319318
_publ_section_title
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 Lanthanide(III) Methylsquarates: Synthesis and X-ray Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1045
_journal_page_last               1051
_journal_paper_doi               10.1021/ic000989q
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C15 H13 Eu O11'
_chemical_formula_weight         521.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2b'
_symmetry_space_group_name_H-M   'P b n a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7129(5)
_cell_length_b                   13.1148(12)
_cell_length_c                   15.2529(9)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.91
_cell_measurement_theta_min      10.67
_cell_volume                     1742.9(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1411
_diffrn_reflns_theta_max         62.99
_diffrn_reflns_theta_min         5.80
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    26.324
_exptl_absorpt_correction_T_max  0.3264
_exptl_absorpt_correction_T_min  0.1719
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_description       'trapezoidal needles'
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.512
_refine_diff_density_min         -1.453
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.00115(13)
_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_all   1.136
_refine_ls_goodness_of_fit_obs   1.208
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1339
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.150
_refine_ls_restrained_S_obs      1.204
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_obs          0.0468
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+9.4558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1051
_refine_ls_wR_factor_obs         0.0947
_reflns_number_observed          1069
_reflns_number_total             1411
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000989q_3.cif
_cod_data_source_block           lh9806
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+9.4558P] 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^)+(0.0407P)^2^+9.4558P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4319318