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_7036143
_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 syn
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_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_audit_update_record
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2015-07-31 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.68(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
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_cell_length_c                   15.766(4)
_cell_measurement_reflns_used    1477
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.98
_cell_measurement_theta_min      2.99
_cell_volume                     1626.1(9)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
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_computing_data_reduction
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics    'DIAMOND, Ver. 3.2 (K. Brandenburg, 2014)'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
;
Xcalibur PX kappa-geometry diffractometer with an Onyx 
CCD camera 
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0963
_diffrn_reflns_av_unetI/netI     0.1695
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
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_diffrn_reflns_limit_k_min       -9
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_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10816
_diffrn_reflns_point_group_measured_fraction_full 0.800
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_diffrn_reflns_theta_full        67.680
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_diffrn_reflns_theta_min         2.996
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.986
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
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            colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.849
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4731
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.848
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.509
_reflns_Friedel_fraction_full    0.579
_reflns_Friedel_fraction_max     0.578
_reflns_number_gt                2423
_reflns_number_total             4731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02478a2.cif
_cod_data_source_block           l6sab
_cod_depositor_comments
'Adding full bibliography for 7036143--7036148.cif.'
_cod_database_code               7036143
_shelx_estimated_absorpt_t_min   0.943
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2013-4
_shelx_res_checksum              17799