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_4319319
_publ_section_title
;
 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            'C10 H16 Gd N O14'
_chemical_formula_weight         531.49
_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                 109.372(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.543(2)
_cell_length_b                   8.3964(11)
_cell_length_c                   15.251(2)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.01
_cell_measurement_theta_min      4.74
_cell_volume                     1756.8(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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            2714
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        5.96
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.848
_exptl_absorpt_correction_T_max  0.6167
_exptl_absorpt_correction_T_min  0.4083
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.089
_refine_ls_goodness_of_fit_obs   1.183
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         2294
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.174
_refine_ls_restrained_S_obs      1.179
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_obs          0.0328
_refine_ls_shift/esd_max         0.108
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0898
_refine_ls_wR_factor_obs         0.0729
_reflns_number_observed          1770
_reflns_number_total             2599
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000989q_4.cif
_cod_data_source_block           LH9808m
_cod_depositor_comments
;
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^)+(0.0441P)^2^+0.0000P] 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^)+(0.0441P)^2^+0.0000P] 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        1756.9(4)
_cod_original_formula_sum        'C10 H16 N O14 Gd'
_cod_database_code               4319319