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_7114198
_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 Gd N8 O5 3+,3(N O3 1-),5(H2 O)'
_chemical_formula_sum            'C48 H76 Gd N11 O19'
_chemical_formula_weight         1268.45
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 104.13(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.290(6)
_cell_length_b                   11.271(3)
_cell_length_c                   22.244(6)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.5115
_cell_measurement_theta_min      2.3205
_cell_volume                     5662(3)
_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  0.0131
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33975
_diffrn_reflns_theta_full        28.51
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_T_max  0.472
_exptl_absorpt_correction_T_min  0.382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS (Sheldrick, 1998), R(int)=0.065 before correction'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.6
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         14382
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0194
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+5.4307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0482
_reflns_Friedel_coverage         0.91
_reflns_number_gt                14112
_reflns_number_total             14382
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b202862j.txt
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

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_sg_symbol_H-M      C2
_cod_database_code               7114198