Formation of Two Diverse Classes of Poly(amino-alkoxide) Chelates and Their Mononuclear and Polynuclear Lanthanide(III) Complexes
Marlon K. Thompson; Alan J. Lough; Andrew J. P. White; David J. Williams; Ishenkumba A. Kahwa; Inorganic Chemistry 42 (2003) 4828–4841; doi:10.1021/ic020154a

data_4313936
_publ_section_title
;
 Formation of Two Diverse Classes of Poly(amino-alkoxide) Chelates and
 Their Mononuclear and Polynuclear Lanthanide(III) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4828
_journal_page_last               4841
_journal_paper_doi               10.1021/ic020154a
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C81 H215 Cl14 N20 O93 Tb5'
_chemical_formula_weight         4248.63
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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            2
_cell_length_a                   23.1578(10)
_cell_length_b                   23.1578(10)
_cell_length_c                   14.9189(10)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      11.28
_cell_volume                     8000.8(7)
_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      173(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  0.0890
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_theta_max         60.01
_diffrn_reflns_theta_min         2.96
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.749
_exptl_absorpt_correction_T_max  0.1512
_exptl_absorpt_correction_T_min  0.0365
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       blocks
_exptl_crystal_F_000             4296
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.772
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.00005(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   1.150
_refine_ls_matrix_type           full
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_refine_ls_restrained_S_obs      1.066
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_obs          0.0791
_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^)+(0.1437P)^2^+4.4740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2514
_refine_ls_wR_factor_obs         0.2035
_reflns_number_observed          3861
_reflns_number_total             5867
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020154a_3.cif
_cod_data_source_block           KW0003
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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^)+(0.1437P)^2^+4.4740P] 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^)+(0.1437P)^2^+4.4740P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'C81 H215 N20 O93 Cl14 Tb5'
_cod_database_code               4313936