Controlling the variation of axial water exchange rates in macrocyclic lanthanide(iii) complexesElectronic supplementary information (ESI) available: experimental section. See http://www.rsc.org/suppdata/cc/b2/b202862j/
Aime, Silvio; Barge, Alessandro; Batsanov, Andrei S.; Botta, Mauro; Castelli, Daniela Delli; Fedeli, Franco; Mortillaro, Armando; Parker, David; Puschmann, Horst; Chemical Communications  (2002) 1120–; doi:10.1039/b202862j

data_7114203
_publ_section_title
;
 Controlling the variation of axial water exchange rates in macrocyclic
 lanthanide(iii) complexesElectronic supplementary information (ESI)
 available: experimental section. See
 http://www.rsc.org/suppdata/cc/b2/b202862j/
;
_journal_issue                   10
_journal_name_full               'Chemical Communications'
_journal_page_first              1120
_journal_paper_doi               10.1039/b202862j
_journal_year                    2002
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C48 H66 N8 O5 Pr 3+,3(C F3 O3 S 1-),C2 H6 O,H2 O'
_chemical_formula_sum            'C53 H74 F9 N8 O16 Pr S3'
_chemical_formula_weight         1487.29
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.70(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.148(9)
_cell_length_b                   12.713(4)
_cell_length_c                   32.952(10)
_cell_measurement_reflns_used    986
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      12.0
_cell_volume                     13439(7)
_computing_cell_refinement       'SMART version 5.625 (Bruker, 2001)'
_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.02A (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL version 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL version 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SMART 6000 CCD area detector'
_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  0.0699
_diffrn_reflns_av_sigmaI/netI    0.1031
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            86128
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  0.9099
_exptl_absorpt_correction_T_min  0.8290
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'XPREP (SHELXTL), R(int)=0.080 before correction'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6112
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.359
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.029(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1605
_refine_ls_number_reflns         34025
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0770P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1465
_reflns_Friedel_coverage         0.806
_reflns_number_gt                22804
_reflns_number_total             34025
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b202862j.txt
_cod_data_source_block           9b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        13439(11)
_cod_original_sg_symbol_H-M      I2
_cod_database_code               7114203