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#$Date: 2016-03-24 00:52:43 +0100 (jue 24 de mar de 2016) $
#$Revision: 179544 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/13/4501368.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_4501368
loop_
_publ_author_name
'Banerjee, Subhabrata'
'Dastidar, Parthasarathi'
_publ_section_title
;
 Coordination Polymers in Selective Separation of Cations and Anions: A
 Series of Rarely Observed All Helical Three-Dimensional Coordination
 Polymers Derived from Various Chiral Amino Acid Based
 Bis-pyridyl-bis-amide Ligands
;
_journal_issue                   12
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5592
_journal_paper_doi               10.1021/cg201161q
_journal_volume                  11
_journal_year                    2011
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C34 H40 Br2 Cu N8 O4 2(H2O)'
_chemical_formula_sum            'C34 H44 Br2 Cu N8 O6'
_chemical_formula_weight         884.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   13.0785(10)
_cell_length_b                   13.0785(10)
_cell_length_c                   20.083(3)
_cell_measurement_temperature    100(2)
_cell_volume                     2974.9(5)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury 2.3'
_computing_publication_material  Shelxl-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'Omega scan'
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34640
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    2.617
_exptl_absorpt_correction_T_max  0.7617
_exptl_absorpt_correction_T_min  0.5278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1353
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0229
_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/[σ²(Fo²)+(0.0354P)²+0.6240P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                3277
_reflns_number_total             3499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201161q_si_004.cif
_cod_data_source_block           sb0652j_0m
_cod_original_sg_symbol_H-M      P3(2)21
_cod_database_code               4501368
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'
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
Cu1 Cu 0.61537(3) 0.61537(3) 0.0000 0.02601(11) Uani 1 2 d S
Br1 Br 0.48710(3) 0.74136(3) -0.027190(13) 0.04015(9) Uani 1 1 d .
N1 N 0.70593(18) 0.73723(19) 0.07237(9) 0.0260(4) Uani 1 1 d .
C2 C 0.6446(2) 0.7627(2) 0.11597(11) 0.0293(5) Uani 1 1 d .
H2 H 0.5659 0.7378 0.1067 0.035 Uiso 1 1 calc R
C3 C 0.6936(2) 0.8252(2) 0.17507(12) 0.0303(6) Uani 1 1 d .
C4 C 0.8112(3) 0.8638(3) 0.18724(14) 0.0395(7) Uani 1 1 d .
H4 H 0.8466 0.9034 0.2265 0.047 Uiso 1 1 calc R
C5 C 0.8753(3) 0.8426(3) 0.14033(14) 0.0392(7) Uani 1 1 d .
H5 H 0.9554 0.8713 0.1470 0.047 Uiso 1 1 calc R
C6 C 0.8208(2) 0.7788(2) 0.08318(13) 0.0316(6) Uani 1 1 d .
H6 H 0.8650 0.7648 0.0520 0.038 Uiso 1 1 calc R
N7 N 0.6171(2) 0.8414(2) 0.21659(10) 0.0385(6) Uani 1 1 d .
H7 H 0.5437 0.8037 0.2058 0.046 Uiso 1 1 calc R
C8 C 0.6455(3) 0.9100(2) 0.27229(12) 0.0344(6) Uani 1 1 d .
O9 O 0.74466(19) 0.9676(2) 0.29332(10) 0.0500(6) Uani 1 1 d .
C10 C 0.5391(3) 0.9091(2) 0.30481(12) 0.0355(7) Uani 1 1 d .
H10 H 0.4737 0.8275 0.3079 0.043 Uiso 1 1 calc R
C11 C 0.5002(3) 0.9815(3) 0.26332(13) 0.0435(7) Uani 1 1 d .
H11A H 0.5665 1.0610 0.2588 0.052 Uiso 1 1 calc R
H11B H 0.4793 0.9474 0.2191 0.052 Uiso 1 1 calc R
C12 C 0.3962(3) 0.9883(3) 0.29195(16) 0.0593(9) Uani 1 1 d .
H12 H 0.4112 1.0060 0.3396 0.071 Uiso 1 1 calc R
C13 C 0.3846(5) 1.0867(4) 0.2601(2) 0.0908(14) Uani 1 1 d .
H13A H 0.3722 1.0726 0.2131 0.136 Uiso 1 1 calc R
H13B H 0.4556 1.1606 0.2676 0.136 Uiso 1 1 calc R
H13C H 0.3188 1.0893 0.2794 0.136 Uiso 1 1 calc R
C14 C 0.2826(4) 0.8714(5) 0.2852(3) 0.1011(18) Uani 1 1 d .
H14A H 0.2197 0.8765 0.3067 0.152 Uiso 1 1 calc R
H14B H 0.2918 0.8103 0.3058 0.152 Uiso 1 1 calc R
H14C H 0.2642 0.8534 0.2389 0.152 Uiso 1 1 calc R
N15 N 0.5731(2) 0.9579(2) 0.37141(10) 0.0363(6) Uani 1 1 d .
H15 H 0.6390 1.0225 0.3764 0.044 Uiso 1 1 calc R
C16 C 0.5070(3) 0.9073(2) 0.42528(12) 0.0324(6) Uani 1 1 d .
O17 O 0.4142(2) 0.81322(18) 0.42422(9) 0.0472(5) Uani 1 1 d .
C18 C 0.5544(2) 0.9769(2) 0.48873(11) 0.0282(6) Uani 1 1 d .
C19 C 0.4744(2) 0.9599(2) 0.53845(11) 0.0272(5) Uani 1 1 d .
H19 H 0.3952 0.9047 0.5318 0.033 Uiso 1 1 calc R
N20 N 0.5066(2) 1.02004(19) 0.59603(9) 0.0268(5) Uani 1 1 d .
C21 C 0.6212(2) 1.0982(2) 0.60538(12) 0.0335(6) Uani 1 1 d .
H21 H 0.6442 1.1405 0.6450 0.040 Uiso 1 1 calc R
C22 C 0.7062(3) 1.1183(3) 0.55849(13) 0.0404(7) Uani 1 1 d .
H22 H 0.7853 1.1720 0.5668 0.049 Uiso 1 1 calc R
C23 C 0.6720(3) 1.0574(3) 0.49925(13) 0.0387(7) Uani 1 1 d .
H23 H 0.7276 1.0705 0.4666 0.046 Uiso 1 1 calc R
O24 O 0.6864(3) 0.3053(3) 0.15352(19) 0.0659(9) Uani 1 1 d .
H24A H 0.654(3) 0.315(3) 0.1800(18) 0.051(12) Uiso 1 1 d .
H24B H 0.680(5) 0.333(5) 0.132(3) 0.09(2) Uiso 1 1 d .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
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
N1 Cu1 N1 94.25(11) 4 .
N1 Cu1 N20 88.52(7) 4 3_564
N1 Cu1 N20 175.75(9) . 3_564
N1 Cu1 N20 175.75(9) 4 6_655
N1 Cu1 N20 88.52(7) . 6_655
N20 Cu1 N20 88.90(12) 3_564 6_655
C6 N1 C2 119.0(2) . .
C6 N1 Cu1 121.95(17) . .
C2 N1 Cu1 118.31(17) . .
N1 C2 C3 122.9(2) . .
N1 C2 H2 118.6 . .
C3 C2 H2 118.6 . .
C4 C3 N7 126.2(2) . .
C4 C3 C2 117.7(2) . .
N7 C3 C2 116.1(2) . .
C5 C4 C3 119.0(2) . .
C5 C4 H4 120.5 . .
C3 C4 H4 120.5 . .
C4 C5 C6 120.4(3) . .
C4 C5 H5 119.8 . .
C6 C5 H5 119.8 . .
N1 C6 C5 120.9(2) . .
N1 C6 H6 119.5 . .
C5 C6 H6 119.5 . .
C8 N7 C3 127.5(3) . .
C8 N7 H7 116.2 . .
C3 N7 H7 116.2 . .
O9 C8 N7 123.5(3) . .
O9 C8 C10 123.1(2) . .
N7 C8 C10 113.4(3) . .
N15 C10 C11 110.7(2) . .
N15 C10 C8 108.1(2) . .
C11 C10 C8 110.2(2) . .
N15 C10 H10 109.2 . .
C11 C10 H10 109.2 . .
C8 C10 H10 109.2 . .
C12 C11 C10 114.5(2) . .
C12 C11 H11A 108.6 . .
C10 C11 H11A 108.6 . .
C12 C11 H11B 108.6 . .
C10 C11 H11B 108.6 . .
H11A C11 H11B 107.6 . .
C13 C12 C14 110.9(4) . .
C13 C12 C11 111.3(3) . .
C14 C12 C11 111.3(3) . .
C13 C12 H12 107.7 . .
C14 C12 H12 107.7 . .
C11 C12 H12 107.7 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C16 N15 C10 123.2(2) . .
C16 N15 H15 118.4 . .
C10 N15 H15 118.4 . .
O17 C16 N15 123.7(2) . .
O17 C16 C18 121.6(2) . .
N15 C16 C18 114.6(2) . .
C23 C18 C19 118.6(2) . .
C23 C18 C16 123.8(2) . .
C19 C18 C16 117.7(2) . .
N20 C19 C18 122.5(2) . .
N20 C19 H19 118.7 . .
C18 C19 H19 118.7 . .
C21 N20 C19 118.1(2) . .
C21 N20 Cu1 120.17(17) . 2_665
C19 N20 Cu1 121.65(18) . 2_665
N20 C21 C22 122.6(2) . .
N20 C21 H21 118.7 . .
C22 C21 H21 118.7 . .
C23 C22 C21 118.8(3) . .
C23 C22 H22 120.6 . .
C21 C22 H22 120.6 . .
C22 C23 C18 119.4(2) . .
C22 C23 H23 120.3 . .
C18 C23 H23 120.3 . .
H24A O24 H24B 98(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.041(2) 4
Cu1 N1 2.041(2) .
Cu1 N20 2.051(2) 3_564
Cu1 N20 2.051(2) 6_655
N1 C6 1.335(3) .
N1 C2 1.338(3) .
C2 C3 1.402(3) .
C2 H2 0.9300 .
C3 C4 1.379(4) .
C3 N7 1.397(3) .
C4 C5 1.378(4) .
C4 H4 0.9300 .
C5 C6 1.388(4) .
C5 H5 0.9300 .
C6 H6 0.9300 .
N7 C8 1.365(3) .
N7 H7 0.8600 .
C8 O9 1.204(4) .
C8 C10 1.532(4) .
C10 N15 1.453(3) .
C10 C11 1.527(4) .
C10 H10 0.9800 .
C11 C12 1.519(5) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C13 1.510(5) .
C12 C14 1.514(7) .
C12 H12 0.9800 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
N15 C16 1.335(3) .
N15 H15 0.8600 .
C16 O17 1.222(3) .
C16 C18 1.507(3) .
C18 C23 1.378(4) .
C18 C19 1.381(3) .
C19 N20 1.342(3) .
C19 H19 0.9300 .
N20 C21 1.339(4) .
N20 Cu1 2.051(2) 2_665
C21 C22 1.379(4) .
C21 H21 0.9300 .
C22 C23 1.376(4) .
C22 H22 0.9300 .
C23 H23 0.9300 .
O24 H24A 0.73(4) .
O24 H24B 0.60(5) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7 O24 0.86 1.95 2.798(4) 170.1 5_565
O24 H24B Br1 0.60(5) 2.74(5) 3.301(4) 157(7) 4
