Metal induced folding: synthesis and conformational analysis of the lanthanide complexes of two 44-membered hydrazone macrocycles.
Klein, Jörg M; Clegg, Jack K.; Saggiomo, Vittorio; Reck, Lisa; Lüning, Ulrich; Sanders, Jeremy K. M.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 3780–3786; doi:10.1039/c2dt11861k

data_7018373
_publ_section_title
;
 Metal induced folding: synthesis and conformational analysis of the
 lanthanide complexes of two 44-membered hydrazone macrocycles.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3780
_journal_page_last               3786
_journal_paper_doi               10.1039/c2dt11861k
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C174 H178 Cl9 Eu3 N36 O30, 17(H2 O)'
_chemical_formula_sum            'C174 H178 Cl9 Eu3 N36 O47'
_chemical_formula_weight         4300.45
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.55(3)
_cell_angle_beta                 87.57(3)
_cell_angle_gamma                76.21(3)
_cell_formula_units_Z            2
_cell_length_a                   15.344(3)
_cell_length_b                   22.768(5)
_cell_length_c                   36.352(7)
_cell_measurement_reflns_used    77765
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      19.98
_cell_measurement_theta_min      1.00
_cell_volume                     12129(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis 2007)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_sigmaI/netI    0.3534
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25417
_diffrn_reflns_theta_full        17.23
_diffrn_reflns_theta_max         17.23
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4384
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.320
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1178
_refine_ls_number_reflns         13368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1766
_refine_ls_R_factor_gt           0.0951
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2745
_refine_ls_wR_factor_ref         0.3112
_reflns_number_gt                4804
_reflns_number_total             13368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt11861k.txt
_cod_data_source_block           new
_cod_original_cell_volume        12129(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7018373