Attempted Syntheses of Lanthanide(III) Complexes of the Anisole- and Anilinosquarate Ligands
Patrice M. T. Piggot; Lincoln A. Hall; Andrew J. P. White; David J. Williams; Inorganic Chemistry 42 (2003) 8344–8352; doi:10.1021/ic034922p

data_4312720
_publ_section_title
;
 Attempted Syntheses of Lanthanide(III) Complexes of the Anisole- and
 Anilinosquarate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8344
_journal_page_last               8352
_journal_paper_doi               10.1021/ic034922p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C33 H34.5 Gd O18.75'
_chemical_formula_weight         888.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 108.6525(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.9313(5)
_cell_length_b                   13.5738(3)
_cell_length_c                   19.5825(3)
_cell_measurement_temperature    150(2)
_cell_volume                     7034.4(2)
_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      150(2)
_diffrn_measurement_device       'Nonius Kappa CCD'
_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  0.0844
_diffrn_reflns_av_sigmaI/netI    0.0972
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47510
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  0.8910
_exptl_absorpt_correction_T_min  0.7981
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       prisms
_exptl_crystal_F_000             3572
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.00036(4)
_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   1.175
_refine_ls_goodness_of_fit_obs   1.344
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         14247
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.196
_refine_ls_restrained_S_obs      1.350
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_obs          0.0649
_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^)+(0.0000P)^2^+45.8763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1473
_refine_ls_wR_factor_obs         0.1264
_reflns_number_observed          9684
_reflns_number_total             16084
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic034922psi20030801_060640_3.cif
_cod_data_source_block           Compound3
_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.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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^)+(0.0000P)^2^+45.8763P] 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^)+(0.0000P)^2^+45.8763P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C33 H34.50 O18.75 Gd'
_cod_database_code               4312720