#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:51:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179309 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/06/4320659.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320659
loop_
_publ_author_name
'Paloma Arranz'
'Carla Bazzicalupi'
'Andrea Bencini'
'Antonio Bianchi'
'Samuele Ciattini'
'Patrizia Fornasari'
'Claudia Giorgi'
'Barbara Valtancoli'
_publ_section_title
;
 Cd(II) and Pb(II) Complexation by Dipyridine-Containing Macrocycles with
 Different Molecular Architecture. Effect of Complex Protonation on Metal
 Coordination Environment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6383
_journal_page_last               6389
_journal_paper_doi               10.1021/ic010597z
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety
;
(Cd 2+), (Br -1)2, (C20 H31 N7 Cd Br2)2, (H2 O)3
;
_chemical_formula_sum            'C40 H68 Br6 Cd3 N14 O3'
_chemical_formula_weight         1609.74
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 117.37(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.504(9)
_cell_length_b                   21.9400(10)
_cell_length_c                   15.7260(10)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    298
_cell_measurement_theta_max      10.0
_cell_measurement_theta_min      7.0
_cell_volume                     5363(4)
_computing_cell_refinement       'ENRAF NONIUS CAD4'
_computing_data_collection       'ENRAF NONIUS CAD4'
_computing_data_reduction        'ENRAF NONIUS CAD4'
_computing_molecular_graphics    'ORTEP-3 (Ver. 1.01β) (Farrugia, 1997)'
_computing_publication_material  'PARST97 (Nardelli, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ENRAF NONIUS CAD4'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1245
_diffrn_reflns_av_sigmaI/netI    0.3134
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3426
_diffrn_reflns_theta_full        21.99
_diffrn_reflns_theta_max         21.99
_diffrn_reflns_theta_min         2.54
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.699
_exptl_absorpt_correction_T_max  0.57
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.994
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.978
_refine_diff_density_min         -1.587
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.2832
_refine_ls_R_factor_gt           0.0972
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1906P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2591
_refine_ls_wR_factor_ref         0.3473
_reflns_number_gt                1349
_reflns_number_total             3279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010597z_1.cif
_cod_data_source_block           '[CdBr2(CdLBr2)2].2H2O'
_cod_original_cell_volume        5363(3)
_cod_database_code               4320659
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.25884(14) 0.42016(11) 0.51671(17) 0.0328(7) Uani 1 1 d . . .
Cd2 Cd 0.5000 0.23276(14) 0.2500 0.0326(10) Uani 1 2 d S . .
Br1 Br 0.4174(3) 0.1543(2) 0.1070(4) 0.0883(17) Uani 1 1 d . . .
Br2 Br 0.3492(4) 0.3227(2) 0.6078(4) 0.0983(19) Uani 1 1 d . . .
Br3 Br 0.2682(4) 0.4732(3) 0.3737(4) 0.105(2) Uani 1 1 d . . .
N1 N 0.3739(16) 0.2619(10) 0.2623(18) 0.030(6) Uani 1 1 d . . .
C1 C 0.291(2) 0.2516(16) 0.194(3) 0.054(10) Uiso 1 1 d . . .
H1 H 0.2806 0.2317 0.1371 0.065 Uiso 1 1 calc . . .
C2 C 0.2187(19) 0.2717(14) 0.209(2) 0.034(8) Uiso 1 1 d . . .
H2 H 0.1631 0.2611 0.1641 0.041 Uiso 1 1 calc . . .
C3 C 0.2311(19) 0.3069(14) 0.289(2) 0.033(8) Uiso 1 1 d . . .
C4 C 0.3186(18) 0.3184(12) 0.350(2) 0.026(7) Uiso 1 1 d . . .
H4 H 0.3312 0.3426 0.4036 0.031 Uiso 1 1 calc . . .
C5 C 0.3838(16) 0.2985(12) 0.3395(19) 0.019(6) Uiso 1 1 d . . .
C6 C 0.481(2) 0.3141(14) 0.414(2) 0.036(8) Uiso 1 1 d . . .
N2 N 0.5368(16) 0.3061(10) 0.381(2) 0.038(7) Uani 1 1 d . . .
C7 C 0.6187(18) 0.3207(12) 0.443(2) 0.026(7) Uiso 1 1 d . . .
H7 H 0.6629 0.3118 0.4273 0.031 Uiso 1 1 calc . . .
C8 C 0.6365(17) 0.3483(12) 0.5267(19) 0.022(7) Uiso 1 1 d . . .
H8 H 0.6916 0.3632 0.5646 0.026 Uiso 1 1 calc . . .
C9 C 0.574(2) 0.3549(14) 0.558(2) 0.040(8) Uiso 1 1 d . . .
C10 C 0.4987(17) 0.3361(12) 0.502(2) 0.022(7) Uiso 1 1 d . . .
H10 H 0.4557 0.3374 0.5212 0.027 Uiso 1 1 calc . . .
C11 C 0.5995(19) 0.3811(13) 0.660(2) 0.032(8) Uiso 1 1 d . . .
H11A H 0.6171 0.3477 0.7056 0.038 Uiso 1 1 calc . . .
H11B H 0.6485 0.4080 0.6783 0.038 Uiso 1 1 calc . . .
N3 N 0.5327(13) 0.4134(10) 0.6661(16) 0.025(6) Uiso 1 1 d . . .
C12 C 0.492(2) 0.4602(15) 0.593(2) 0.045(9) Uiso 1 1 d . . .
H12A H 0.4559 0.4401 0.5326 0.054 Uiso 1 1 calc . . .
H12B H 0.5366 0.4818 0.5851 0.054 Uiso 1 1 calc . . .
C13 C 0.436(2) 0.5079(14) 0.612(2) 0.038(8) Uiso 1 1 d . . .
H13A H 0.4736 0.5347 0.6632 0.045 Uiso 1 1 calc . . .
H13B H 0.4057 0.5325 0.5549 0.045 Uiso 1 1 calc . . .
N4 N 0.3728(15) 0.4798(10) 0.6384(17) 0.027(6) Uani 1 1 d . . .
H4A H 0.4025 0.4546 0.6890 0.032 Uiso 1 1 calc . . .
C14 C 0.332(2) 0.5261(15) 0.670(3) 0.049(9) Uiso 1 1 d . . .
H14A H 0.3743 0.5573 0.7048 0.058 Uiso 1 1 calc . . .
H14B H 0.3147 0.5076 0.7147 0.058 Uiso 1 1 calc . . .
C15 C 0.254(2) 0.5561(17) 0.590(3) 0.057(10) Uiso 1 1 d . . .
H15A H 0.2282 0.5845 0.6162 0.068 Uiso 1 1 calc . . .
H15B H 0.2715 0.5786 0.5484 0.068 Uiso 1 1 calc . . .
N5 N 0.1921(18) 0.5101(12) 0.535(2) 0.048(8) Uiso 1 1 d . . .
H5 H 0.1604 0.5257 0.4749 0.058 Uiso 1 1 calc . . .
C16 C 0.133(2) 0.4984(15) 0.574(3) 0.049(9) Uiso 1 1 d . . .
H16A H 0.0930 0.5323 0.5596 0.058 Uiso 1 1 calc . . .
H16B H 0.1643 0.4941 0.6430 0.058 Uiso 1 1 calc . . .
C17 C 0.084(3) 0.4415(18) 0.531(3) 0.067(12) Uiso 1 1 d . . .
H17A H 0.0453 0.4332 0.5584 0.080 Uiso 1 1 calc . . .
H17B H 0.0495 0.4471 0.4628 0.080 Uiso 1 1 calc . . .
N6 N 0.1439(16) 0.3871(12) 0.549(2) 0.048(8) Uani 1 1 d . . .
H6 H 0.1682 0.3797 0.6135 0.057 Uiso 1 1 calc . . .
C18 C 0.107(3) 0.3310(18) 0.503(3) 0.065(12) Uiso 1 1 d . . .
H18A H 0.0530 0.3243 0.5046 0.079 Uiso 1 1 calc . . .
H18B H 0.1456 0.2976 0.5373 0.079 Uiso 1 1 calc . . .
C19 C 0.093(2) 0.3326(13) 0.405(2) 0.035(8) Uiso 1 1 d . . .
H19A H 0.0602 0.2969 0.3721 0.042 Uiso 1 1 calc . . .
H19B H 0.0589 0.3682 0.3741 0.042 Uiso 1 1 calc . . .
N7 N 0.1697(17) 0.3342(11) 0.393(2) 0.046(8) Uani 1 1 d . . .
H7A H 0.1976 0.2993 0.4219 0.055 Uiso 1 1 calc . . .
C20 C 0.159(2) 0.3289(14) 0.300(2) 0.037(8) Uiso 1 1 d . . .
H20A H 0.1437 0.3687 0.2695 0.044 Uiso 1 1 calc . . .
H20B H 0.1109 0.3019 0.2643 0.044 Uiso 1 1 calc . . .
O1 O 0.172(2) 0.4021(15) 0.759(2) 0.100(11) Uiso 1 1 d . . .
O2 O 0.5000 -0.009(3) 0.2500 0.20(3) Uiso 1 2 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Cd1 N6 73.7(9) . . ?
N5 Cd1 N4 74.2(9) . . ?
N6 Cd1 N4 117.4(9) . . ?
N5 Cd1 Br3 87.8(7) . . ?
N6 Cd1 Br3 135.2(7) . . ?
N4 Cd1 Br3 94.9(5) . . ?
N5 Cd1 N7 121.6(9) . . ?
N6 Cd1 N7 70.9(9) . . ?
N4 Cd1 N7 164.2(8) . . ?
Br3 Cd1 N7 86.2(6) . . ?
N5 Cd1 Br2 144.0(7) . . ?
N6 Cd1 Br2 89.5(6) . . ?
N4 Cd1 Br2 86.5(5) . . ?
Br3 Cd1 Br2 124.6(2) . . ?
N7 Cd1 Br2 80.0(6) . . ?
N1 Cd2 N1 149.0(10) . 2_655 ?
N1 Cd2 N2 69.6(8) . . ?
N1 Cd2 N2 89.9(8) 2_655 . ?
N1 Cd2 N2 89.9(8) . 2_655 ?
N1 Cd2 N2 69.6(8) 2_655 2_655 ?
N2 Cd2 N2 98.3(11) . 2_655 ?
N1 Cd2 Br1 94.5(6) . . ?
N1 Cd2 Br1 105.5(6) 2_655 . ?
N2 Cd2 Br1 164.0(6) . . ?
N2 Cd2 Br1 83.3(6) 2_655 . ?
N1 Cd2 Br1 105.5(6) . 2_655 ?
N1 Cd2 Br1 94.5(6) 2_655 2_655 ?
N2 Cd2 Br1 83.3(6) . 2_655 ?
N2 Cd2 Br1 164.0(6) 2_655 2_655 ?
Br1 Cd2 Br1 99.7(3) . 2_655 ?
C1 N1 C5 116(2) . . ?
C1 N1 Cd2 125(2) . . ?
C5 N1 Cd2 118.3(18) . . ?
N1 C1 C2 120(3) . . ?
C3 C2 C1 122(3) . . ?
C4 C3 C2 112(3) . . ?
C4 C3 C20 127(3) . . ?
C2 C3 C20 121(3) . . ?
C5 C4 C3 127(3) . . ?
C4 C5 N1 123(3) . . ?
C4 C5 C6 122(3) . . ?
N1 C5 C6 115(2) . . ?
N2 C6 C10 126(3) . . ?
N2 C6 C5 115(3) . . ?
C10 C6 C5 119(3) . . ?
C6 N2 C7 115(3) . . ?
C6 N2 Cd2 118(2) . . ?
C7 N2 Cd2 122.6(19) . . ?
N2 C7 C8 120(3) . . ?
C7 C8 C9 122(3) . . ?
C10 C9 C8 117(3) . . ?
C10 C9 C11 123(3) . . ?
C8 C9 C11 120(3) . . ?
C9 C10 C6 120(3) . . ?
N3 C11 C9 114(3) . . ?
C11 N3 C12 115(2) . . ?
N3 C12 C13 116(3) . . ?
N4 C13 C12 113(2) . . ?
C14 N4 C13 111(2) . . ?
C14 N4 Cd1 107.2(19) . . ?
C13 N4 Cd1 116.9(18) . . ?
N4 C14 C15 114(3) . . ?
N5 C15 C14 110(3) . . ?
C15 N5 C16 111(3) . . ?
C15 N5 Cd1 112(2) . . ?
C16 N5 Cd1 113(2) . . ?
N5 C16 C17 109(3) . . ?
N6 C17 C16 112(3) . . ?
C18 N6 C17 118(3) . . ?
C18 N6 Cd1 112(2) . . ?
C17 N6 Cd1 107(2) . . ?
N6 C18 C19 110(3) . . ?
N7 C19 C18 115(3) . . ?
C20 N7 C19 117(3) . . ?
C20 N7 Cd1 125(2) . . ?
C19 N7 Cd1 101.1(18) . . ?
N7 C20 C3 117(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N5 2.37(3) . ?
Cd1 N6 2.41(3) . ?
Cd1 N4 2.42(3) . ?
Cd1 Br3 2.602(6) . ?
Cd1 N7 2.64(3) . ?
Cd1 Br2 2.653(6) . ?
Cd2 N1 2.39(2) . ?
Cd2 N1 2.39(2) 2_655 ?
Cd2 N2 2.46(3) . ?
Cd2 N2 2.46(3) 2_655 ?
Cd2 Br1 2.668(5) . ?
Cd2 Br1 2.668(5) 2_655 ?
N1 C1 1.37(4) . ?
N1 C5 1.40(3) . ?
C1 C2 1.45(5) . ?
C2 C3 1.41(4) . ?
C3 C4 1.41(4) . ?
C3 C20 1.43(4) . ?
C4 C5 1.30(4) . ?
C5 C6 1.60(4) . ?
C6 N2 1.31(4) . ?
C6 C10 1.36(4) . ?
N2 C7 1.35(4) . ?
C7 C8 1.35(4) . ?
C8 C9 1.40(4) . ?
C9 C10 1.27(4) . ?
C9 C11 1.56(4) . ?
C11 N3 1.41(3) . ?
N3 C12 1.46(4) . ?
C12 C13 1.55(4) . ?
C13 N4 1.49(4) . ?
N4 C14 1.45(4) . ?
C14 C15 1.52(5) . ?
C15 N5 1.44(4) . ?
N5 C16 1.46(4) . ?
C16 C17 1.49(5) . ?
C17 N6 1.53(4) . ?
N6 C18 1.42(5) . ?
C18 C19 1.45(5) . ?
C19 N7 1.43(4) . ?
N7 C20 1.40(4) . ?
