Lanthanide(iii) and lead(ii) complexes of a chiral nonaaza macrocyclic amine based on 1,2-diaminocyclopentane.
Gregoliński, Janusz; Slepokura, Katarzyna; Lisowski, Jerzy; Dalton transactions (Cambridge, England : 2003) 44 (2015) 16345–16351; doi:10.1039/c5dt02478a

data_7036144
_publ_section_title
;
 Lanthanide(iii) and lead(ii) complexes of a chiral nonaaza macrocyclic
 amine based on 1,2-diaminocyclopentane.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16345
_journal_page_last               16351
_journal_paper_doi               10.1039/c5dt02478a
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C36 H51 N9 Pr, 3(N O3), 1.5(C2 H3 N), 1.2(H2 O)'
_chemical_formula_sum            'C39 H57.9 N13.5 O10.2 Pr'
_chemical_formula_weight         1019.99
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-07-31 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   16.139(3)
_cell_length_b                   18.968(6)
_cell_length_c                   46.829(12)
_cell_measurement_reflns_used    26672
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.75
_cell_measurement_theta_min      2.73
_cell_volume                     14336(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'DIAMOND, Ver. 3.2 (K. Brandenburg, 2014)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Xcalibur R kappa-geometry diffractometer with a Ruby 
CCD camera 
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            77426
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.734
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             6324
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.112
_refine_diff_density_min         -2.018
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Flack x determined using 6869 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.012(4)
_refine_ls_extinction_coef       0.00060(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         20901
_refine_ls_number_restraints     221
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0898P)^2^+15.0135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1569
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                17040
_reflns_number_total             20901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02478a2.cif
_cod_data_source_block           prl6snab
_cod_depositor_comments
'Adding full bibliography for 7036143--7036148.cif.'
_cod_original_formula_sum        'C39 H57.90 N13.50 O10.20 Pr'
_cod_database_code               7036144
_shelx_estimated_absorpt_t_min   0.743
_shelx_estimated_absorpt_t_max   0.845
_shelxl_version_number           2013-4
_shelx_res_checksum              97259