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#$Date: 2016-03-26 18:17:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180421 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/90/7209059.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_7209059
loop_
_publ_author_name
'Banerjee, Subhabrata'
'Adrash, N. N.'
'Dastidar, Parthasarathi'
_publ_section_title
;
 Anions as additive and template in tuning metallasupramolecular
 architecture in CuII coordination compounds derived from l-amino acid
 based chiral ligands
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              245
_journal_paper_doi               10.1039/c2ce26475g
_journal_volume                  15
_journal_year                    2013
_chemical_absolute_configuration syn
_chemical_formula_sum            'C112 H132 Br4 Cu4 F12 N32 O26 Si2'
_chemical_formula_weight         3200.48
_chemical_name_systematic
;
?
;
_space_group_IT_number           79
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_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                90.00
_cell_formula_units_Z            1
_cell_length_a                   14.1357(7)
_cell_length_b                   14.1357(7)
_cell_length_c                   17.7983(17)
_cell_measurement_temperature    100(2)
_cell_volume                     3556.4(4)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury 2.4'
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21898
_diffrn_reflns_theta_full        25.57
_diffrn_reflns_theta_max         25.57
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.822
_exptl_absorpt_correction_T_max  0.8679
_exptl_absorpt_correction_T_min  0.6689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3298
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1647P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1935
_refine_ls_wR_factor_ref         0.2046
_reflns_number_gt                2609
_reflns_number_total             3298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26475g.txt
_cod_data_source_block           sb07j_0m
_cod_original_sg_symbol_H-M      I4
_cod_database_code               7209059
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+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
Cu1 Cu 1.0000 1.0000 1.00062(9) 0.0471(4) Uani 1 4 d S
Cu2 Cu 1.0000 1.0000 0.53611(9) 0.0528(4) Uani 1 4 d S
Br1 Br 1.0000 1.0000 0.38536(7) 0.0825(6) Uani 1 4 d S
Si1 Si 1.0000 1.0000 0.7798(2) 0.0522(8) Uani 1 4 d S
F1 F 1.0000 1.0000 0.8750(5) 0.070(2) Uani 1 4 d S
F2 F 0.9409(3) 0.8963(3) 0.7811(2) 0.0645(10) Uani 1 1 d .
F3 F 1.0000 1.0000 0.6865(4) 0.0559(17) Uani 1 4 d S
N1 N 0.9438(4) 0.8702(4) 1.0062(3) 0.0470(11) Uani 1 1 d .
C2 C 0.9647(6) 0.8134(6) 1.0648(4) 0.0636(19) Uani 1 1 d .
H2 H 1.0033 0.8379 1.1023 0.076 Uiso 1 1 calc R
C3 C 0.9338(7) 0.7237(6) 1.0728(5) 0.073(2) Uani 1 1 d .
H3 H 0.9492 0.6890 1.1155 0.087 Uiso 1 1 calc R
C4 C 0.8795(7) 0.6844(6) 1.0175(5) 0.077(2) Uani 1 1 d .
H4 H 0.8598 0.6217 1.0206 0.092 Uiso 1 1 calc R
C5 C 0.8544(4) 0.7402(5) 0.9566(5) 0.0565(15) Uani 1 1 d .
C6 C 0.8878(4) 0.8345(5) 0.9531(4) 0.0532(14) Uani 1 1 d .
H6 H 0.8703 0.8724 0.9127 0.064 Uiso 1 1 calc R
C7 C 0.7968(6) 0.6930(6) 0.8949(4) 0.0678(18) Uani 1 1 d .
O8 O 0.8011(6) 0.6077(4) 0.8887(5) 0.108(2) Uani 1 1 d .
N9 N 0.7424(4) 0.7454(4) 0.8525(3) 0.0635(16) Uani 1 1 d .
H9 H 0.7405 0.8056 0.8594 0.076 Uiso 1 1 calc R
C10 C 0.6857(7) 0.7031(6) 0.7943(5) 0.072(2) Uani 1 1 d .
H10 H 0.6687 0.6395 0.8117 0.086 Uiso 1 1 calc R
C11 C 0.5913(6) 0.7602(8) 0.7870(5) 0.086(3) Uani 1 1 d .
H11A H 0.6055 0.8259 0.7796 0.128 Uiso 1 1 calc R
H11B H 0.5547 0.7526 0.8320 0.128 Uiso 1 1 calc R
H11C H 0.5559 0.7369 0.7448 0.128 Uiso 1 1 calc R
C12 C 0.7307(6) 0.6918(6) 0.7196(4) 0.0636(19) Uani 1 1 d .
O13 O 0.7151(6) 0.6237(5) 0.6814(4) 0.109(3) Uani 1 1 d .
N14 N 0.7887(5) 0.7638(4) 0.6969(4) 0.077(2) Uani 1 1 d .
H14 H 0.7961 0.8097 0.7281 0.092 Uiso 1 1 calc R
C15 C 0.8375(5) 0.7713(5) 0.6285(4) 0.0578(17) Uani 1 1 d .
C16 C 0.8542(7) 0.6971(6) 0.5784(5) 0.073(2) Uani 1 1 d .
H16 H 0.8291 0.6372 0.5869 0.088 Uiso 1 1 calc R
C17 C 0.9072(6) 0.7145(6) 0.5181(5) 0.076(2) Uani 1 1 d .
H17 H 0.9189 0.6655 0.4846 0.091 Uiso 1 1 calc R
C18 C 0.9459(6) 0.8033(6) 0.5032(4) 0.0667(18) Uani 1 1 d .
H18 H 0.9822 0.8123 0.4602 0.080 Uiso 1 1 calc R
N19 N 0.9312(4) 0.8756(4) 0.5504(3) 0.0564(15) Uani 1 1 d .
C20 C 0.8758(5) 0.8606(6) 0.6118(3) 0.0595(18) Uani 1 1 d .
H20 H 0.8628 0.9111 0.6437 0.071 Uiso 1 1 calc R
Br2A Br 1.0312(8) 0.5007(11) 1.1459(8) 0.140(3) Uiso 0.14 1 d P
Br2B Br 1.0376(10) 0.5076(13) 1.1916(12) 0.140(3) Uiso 0.11 1 d P
O1W O 1.0000 1.0000 1.1820(16) 0.134(6) Uiso 1 4 d S
O2A O 0.7413(9) 0.9494(9) 0.8055(7) 0.101(3) Uiso 0.59 1 d P
O2B O 0.6941(12) 0.9411(13) 0.8786(12) 0.101(3) Uiso 0.41 1 d P
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Si Si 0.0817 0.0704 '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'
H H 0.0000 0.0000 '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 174.3(3) . 3_775
N1 Cu1 N1 89.860(17) . 2_755
N1 Cu1 N1 89.859(18) 3_775 2_755
N1 Cu1 N1 89.859(18) . 4_575
N1 Cu1 N1 89.856(17) 3_775 4_575
N1 Cu1 N1 174.3(3) 2_755 4_575
N1 Cu1 F1 92.85(16) . .
N1 Cu1 F1 92.85(16) 3_775 .
N1 Cu1 F1 92.85(16) 2_755 .
N1 Cu1 F1 92.85(16) 4_575 .
N19 Cu2 N19 89.10(4) . 2_755
N19 Cu2 N19 165.6(3) . 3_775
N19 Cu2 N19 89.10(4) 2_755 3_775
N19 Cu2 N19 89.10(4) . 4_575
N19 Cu2 N19 165.6(3) 2_755 4_575
N19 Cu2 N19 89.10(4) 3_775 4_575
N19 Cu2 Br1 97.21(15) . .
N19 Cu2 Br1 97.21(15) 2_755 .
N19 Cu2 Br1 97.21(15) 3_775 .
N19 Cu2 Br1 97.21(15) 4_575 .
F3 Si1 F2 90.78(17) . 2_755
F3 Si1 F2 90.78(17) . 3_775
F2 Si1 F2 89.986(6) 2_755 3_775
F3 Si1 F2 90.78(17) . 4_575
F2 Si1 F2 178.4(3) 2_755 4_575
F2 Si1 F2 89.990(5) 3_775 4_575
F3 Si1 F2 90.78(17) . .
F2 Si1 F2 89.990(6) 2_755 .
F2 Si1 F2 178.4(3) 3_775 .
F2 Si1 F2 89.991(6) 4_575 .
F3 Si1 F1 180.000(3) . .
F2 Si1 F1 89.22(17) 2_755 .
F2 Si1 F1 89.22(17) 3_775 .
F2 Si1 F1 89.22(17) 4_575 .
F2 Si1 F1 89.22(17) . .
Si1 F1 Cu1 180.000(1) . .
C6 N1 C2 117.0(6) . .
C6 N1 Cu1 123.2(4) . .
C2 N1 Cu1 119.8(5) . .
N1 C2 C3 124.8(7) . .
N1 C2 H2 117.6 . .
C3 C2 H2 117.6 . .
C2 C3 C4 119.2(7) . .
C2 C3 H3 120.4 . .
C4 C3 H3 120.4 . .
C3 C4 C5 118.4(7) . .
C3 C4 H4 120.8 . .
C5 C4 H4 120.8 . .
C4 C5 C6 119.0(7) . .
C4 C5 C7 116.8(6) . .
C6 C5 C7 124.0(7) . .
N1 C6 C5 121.6(6) . .
N1 C6 H6 119.2 . .
C5 C6 H6 119.2 . .
O8 C7 N9 122.7(8) . .
O8 C7 C5 118.4(8) . .
N9 C7 C5 118.9(7) . .
C7 N9 C10 120.5(7) . .
C7 N9 H9 119.7 . .
C10 N9 H9 119.8 . .
N9 C10 C12 116.8(7) . .
N9 C10 C11 108.7(7) . .
C12 C10 C11 110.3(7) . .
N9 C10 H10 106.9 . .
C12 C10 H10 106.9 . .
C11 C10 H10 106.9 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
O13 C12 N14 122.6(8) . .
O13 C12 C10 121.1(8) . .
N14 C12 C10 116.3(7) . .
C12 N14 C15 127.4(6) . .
C12 N14 H14 116.3 . .
C15 N14 H14 116.3 . .
C16 C15 N14 125.5(7) . .
C16 C15 C20 118.3(7) . .
N14 C15 C20 116.1(6) . .
C17 C16 C15 118.1(8) . .
C17 C16 H16 121.0 . .
C15 C16 H16 121.0 . .
C16 C17 C18 122.8(7) . .
C16 C17 H17 118.6 . .
C18 C17 H17 118.6 . .
N19 C18 C17 120.5(7) . .
N19 C18 H18 119.8 . .
C17 C18 H18 119.8 . .
C18 N19 C20 118.3(7) . .
C18 N19 Cu2 120.7(5) . .
C20 N19 Cu2 120.8(5) . .
N19 C20 C15 122.1(7) . .
N19 C20 H20 119.0 . .
C15 C20 H20 119.0 . .
Br2B Br2A Br2A 96.5(15) . 3_765
Br2B Br2A Br2B 57.5(18) . 3_765
Br2A Br2A Br2B 40.1(8) 3_765 3_765
Br2A Br2B Br2B 82.5(15) . 3_765
Br2A Br2B Br2A 43.5(15) . 3_765
Br2B Br2B Br2A 40.0(8) 3_765 3_765
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.002(5) .
Cu1 N1 2.002(5) 3_775
Cu1 N1 2.002(5) 2_755
Cu1 N1 2.002(5) 4_575
Cu1 F1 2.236(8) .
Cu2 N19 2.025(6) .
Cu2 N19 2.025(6) 2_755
Cu2 N19 2.025(6) 3_775
Cu2 N19 2.025(6) 4_575
Cu2 Br1 2.683(2) .
Si1 F3 1.661(9) .
Si1 F2 1.688(4) 2_755
Si1 F2 1.688(4) 3_775
Si1 F2 1.688(4) 4_575
Si1 F2 1.688(4) .
Si1 F1 1.694(8) .
N1 C6 1.333(9) .
N1 C2 1.348(9) .
C2 C3 1.349(13) .
C2 H2 0.9300 .
C3 C4 1.366(13) .
C3 H3 0.9300 .
C4 C5 1.387(11) .
C4 H4 0.9300 .
C5 C6 1.416(10) .
C5 C7 1.521(11) .
C6 H6 0.9300 .
C7 O8 1.213(10) .
C7 N9 1.307(10) .
N9 C10 1.440(10) .
N9 H9 0.8600 .
C10 C12 1.482(12) .
C10 C11 1.564(14) .
C10 H10 0.9800 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 O13 1.199(10) .
C12 N14 1.369(11) .
N14 C15 1.403(10) .
N14 H14 0.8600 .
C15 C16 1.397(11) .
C15 C20 1.406(11) .
C16 C17 1.331(13) .
C16 H16 0.9300 .
C17 C18 1.394(13) .
C17 H17 0.9300 .
C18 N19 1.339(10) .
C18 H18 0.9300 .
N19 C20 1.362(9) .
C20 H20 0.9300 .
Br2A Br2B 0.82(2) .
Br2A Br2A 0.88(2) 3_765
Br2A Br2B 1.273(18) 3_765
Br2B Br2B 1.08(3) 3_765
Br2B Br2A 1.273(18) 3_765
O2A O2B 1.47(2) .
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
C2 H2 O13 0.93 2.33 3.086(10) 138.0 8_565
