Structural Analysis of Nine-Coordinate Lanthanide Complexes: Steric Control of the Metal-Water Distance Across the Series
David Parker; Horst Puschmann; Andrei S. Batsanov; Kanthi Senanayake; Inorganic Chemistry 42 (2003) 8646–8651; doi:10.1021/ic030203z

data_4312753
_publ_contact_author             'Andrei S.Batsanov'
_publ_contact_author_email       a.s.batsanov@durham.ac.uk
_publ_section_title
;
 Structural Analysis of Nine-Coordinate Lanthanide Complexes: Steric
 Control of the Metal-Water Distance Across the Series
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8646
_journal_page_last               8651
_journal_paper_doi               10.1021/ic030203z
_journal_volume                  42
_journal_year                    2003
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H66 Gd N8 O5 3+,3(C F3 O3 S 1-),3(H2 O)'
_chemical_formula_sum            'C51 H72 F9 Gd N8 O17 S3'
_chemical_formula_weight         1493.60
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.78(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.666(3)
_cell_length_b                   11.674(2)
_cell_length_c                   19.236(4)
_cell_measurement_reflns_used    7381
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      2.33
_cell_volume                     3224.0(11)
_computing_cell_refinement       'SMART version 5.625 (Bruker, 2001)'
_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.28A (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL version 5.10 (Bruker, 1997)'
_computing_publication_material  'SHELXTL version 5.10 (Bruker, 1997)'
_computing_structure_refinement  'SHELXTL version 6.12 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL version 6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'APEX CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
'60W microfocus Bede Microsource with glass polycapillary optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48792
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    1.222
_exptl_absorpt_correction_T_max  0.8875
_exptl_absorpt_correction_T_min  0.8171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS v.2.03 (Sheldrick,2001), R(int)=0.031 before correction'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'oblique block'
_exptl_crystal_F_000             1526
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         18404
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+1.1663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0667
_reflns_Friedel_coverage         0.886
_reflns_number_gt                17488
_reflns_number_total             18404
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic030203z_6.cif
_cod_data_source_block           02srv258R
_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 
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_cod_database_code               4312753