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_4319316
_publ_section_title
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 Lanthanide(III) Methylsquarates: Synthesis and X-ray Structures
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_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            'C10 H16 N O14 Tb'
_chemical_formula_weight         533.16
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 109.428(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.574(2)
_cell_length_b                   8.3967(11)
_cell_length_c                   15.272(2)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.51
_cell_measurement_theta_min      5.31
_cell_volume                     1762.5(4)
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3222
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.72
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.085
_exptl_absorpt_correction_T_max  0.6885
_exptl_absorpt_correction_T_min  0.4596
_exptl_absorpt_correction_type   'Face-indexed numerical'
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.932
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.0009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_goodness_of_fit_obs   1.127
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2772
_refine_ls_number_restraints     11
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_refine_ls_restrained_S_obs      1.124
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_obs          0.0327
_refine_ls_shift/esd_max         -0.040
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.7443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0874
_refine_ls_wR_factor_obs         0.0742
_reflns_number_observed          2104
_reflns_number_total             3092
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000989q_1.cif
_cod_data_source_block           LH0001
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0430P)^2^+0.7443P] 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^)+(0.0430P)^2^+0.7443P] 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        1762.4(4)
_cod_database_code               4319316