#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:29:24 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180476 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/45/7214542.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_7214542
loop_
_publ_author_name
'Banerjee, Subhabrata'
'Dastidar, Parthasarathi'
_publ_section_title
;
 Studying fluorous interactions in a series of coordination compounds
 derived from mono-pyridyl ligands equipped with hydrogen bonding
 functionality: exploiting anion⋯\pF interaction in separating
 ClO4− anion from a competing mixture of anions
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              9415
_journal_paper_doi               10.1039/c3ce40359a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C48 H45 Cu N12 O15 S'
_chemical_formula_weight         1137.56
_chemical_name_systematic
;
?
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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            2
_cell_length_a                   17.8802(14)
_cell_length_b                   17.8802(14)
_cell_length_c                   8.4406(9)
_cell_measurement_temperature    298(2)
_cell_volume                     2698.5(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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0659
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            27596
_diffrn_reflns_theta_full        24.19
_diffrn_reflns_theta_max         24.19
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.9261
_exptl_absorpt_correction_T_min  0.8596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.711
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.812
_refine_ls_shift/su_mean         0.053
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1094P)²+16.7802P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2371
_refine_ls_wR_factor_ref         0.2412
_reflns_number_gt                1943
_reflns_number_total             2172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40359a.txt
_cod_data_source_block           y_CC9
_cod_original_sg_symbol_H-M      P4/n
_cod_database_code               7214542
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
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 0.2500 0.2500 0.27148(17) 0.0203(5) Uani 1 4 d S
S1 S 0.7500 0.2500 0.5000 0.0211(7) Uani 1 4 d S
N1 N 0.2672(2) 0.3631(3) 0.2642(6) 0.0221(11) Uani 1 1 d .
C2 C 0.2392(3) 0.4081(3) 0.3751(8) 0.0244(13) Uani 1 1 d .
H2 H 0.2120 0.3872 0.4579 0.029 Uiso 1 1 calc R
C3 C 0.2490(3) 0.4852(3) 0.3716(8) 0.0251(13) Uani 1 1 d .
C4 C 0.2860(3) 0.5157(3) 0.2431(8) 0.0299(14) Uani 1 1 d .
H4 H 0.2917 0.5672 0.2352 0.036 Uiso 1 1 calc R
C5 C 0.3141(3) 0.4699(3) 0.1275(8) 0.0312(15) Uani 1 1 d .
H5 H 0.3387 0.4900 0.0403 0.037 Uiso 1 1 calc R
C6 C 0.3054(3) 0.3935(3) 0.1421(8) 0.0271(13) Uani 1 1 d .
H6 H 0.3263 0.3623 0.0661 0.033 Uiso 1 1 calc R
N7 N 0.2224(3) 0.5353(3) 0.4886(6) 0.0292(12) Uani 1 1 d .
H7 H 0.2219 0.5821 0.4644 0.035 Uiso 1 1 calc R
C8 C 0.1978(4) 0.5167(3) 0.6342(8) 0.0311(15) Uani 1 1 d .
O9 O 0.1984(3) 0.4519(3) 0.6866(6) 0.0499(14) Uani 1 1 d .
N10 N 0.1743(3) 0.5765(3) 0.7204(6) 0.0292(12) Uani 1 1 d .
H10 H 0.1737 0.6193 0.6737 0.035 Uiso 1 1 calc R
C11 C 0.1506(3) 0.5745(3) 0.8797(8) 0.0294(14) Uani 1 1 d .
C12 C 0.1135(4) 0.5146(4) 0.9472(9) 0.0360(16) Uani 1 1 d .
H12 H 0.1050 0.4714 0.8883 0.043 Uiso 1 1 calc R
C13 C 0.0893(4) 0.5188(4) 1.1013(10) 0.0450(18) Uani 1 1 d .
H13 H 0.0649 0.4781 1.1464 0.054 Uiso 1 1 calc R
C14 C 0.1005(4) 0.5827(4) 1.1907(9) 0.0413(17) Uani 1 1 d .
H14 H 0.0831 0.5854 1.2944 0.050 Uiso 1 1 calc R
C15 C 0.1382(4) 0.6427(4) 1.1233(9) 0.0373(17) Uani 1 1 d .
H15 H 0.1469 0.6856 1.1829 0.045 Uiso 1 1 calc R
C16 C 0.1625(3) 0.6392(3) 0.9708(8) 0.0288(14) Uani 1 1 d .
H16 H 0.1872 0.6799 0.9265 0.035 Uiso 1 1 calc R
O17 O 0.2500 0.2500 0.5452(11) 0.0278(18) Uani 1 4 d S
H17 H 0.2169 0.2778 0.5776 0.042 Uiso 0.25 1 calc PR
O18 O 0.7234(2) 0.3125(2) 0.5997(6) 0.0342(11) Uani 1 1 d .
O19A O 0.1477(5) 0.3117(5) 0.7517(11) 0.083(3) Uani 0.85 1 d P
O19B O 0.0895(15) 0.3471(18) 0.759(4) 0.036(7) Uani 0.15 1 d P
O20 O 0.2500 0.2500 0.9696(11) 0.035(2) Uani 1 4 d S
O21 O 0.9724(11) 0.5436(11) 0.504(2) 0.041(5) Uiso 0.25 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'
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'
S S 0.1246 0.1234 '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'
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 89.948(9) 2 4
N1 Cu1 N1 89.948(10) 2 3
N1 Cu1 N1 176.5(3) 4 3
N1 Cu1 N1 176.5(3) 2 .
N1 Cu1 N1 89.949(9) 4 .
N1 Cu1 N1 89.947(9) 3 .
N1 Cu1 O17 91.73(15) 2 .
N1 Cu1 O17 91.73(15) 4 .
N1 Cu1 O17 91.73(15) 3 .
N1 Cu1 O17 91.73(15) . .
O18 S1 O18 110.6(4) 8_656 7_666
O18 S1 O18 108.93(19) 8_656 2_655
O18 S1 O18 108.93(19) 7_666 2_655
O18 S1 O18 108.93(19) 8_656 .
O18 S1 O18 108.93(19) 7_666 .
O18 S1 O18 110.6(4) 2_655 .
C2 N1 C6 118.8(5) . .
C2 N1 Cu1 121.3(4) . .
C6 N1 Cu1 119.8(4) . .
N1 C2 C3 122.5(6) . .
N1 C2 H2 118.8 . .
C3 C2 H2 118.8 . .
C4 C3 C2 117.9(6) . .
C4 C3 N7 117.3(5) . .
C2 C3 N7 124.8(6) . .
C5 C4 C3 120.0(6) . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
C4 C5 C6 119.1(6) . .
C4 C5 H5 120.5 . .
C6 C5 H5 120.5 . .
N1 C6 C5 121.6(6) . .
N1 C6 H6 119.2 . .
C5 C6 H6 119.2 . .
C8 N7 C3 126.1(5) . .
C8 N7 H7 116.9 . .
C3 N7 H7 116.9 . .
O9 C8 N7 123.6(6) . .
O9 C8 N10 123.1(6) . .
N7 C8 N10 113.3(5) . .
C8 N10 C11 125.6(5) . .
C8 N10 H10 117.2 . .
C11 N10 H10 117.2 . .
C12 C11 C16 119.0(6) . .
C12 C11 N10 123.8(6) . .
C16 C11 N10 117.1(6) . .
C13 C12 C11 119.9(6) . .
C13 C12 H12 120.0 . .
C11 C12 H12 120.0 . .
C12 C13 C14 121.1(7) . .
C12 C13 H13 119.5 . .
C14 C13 H13 119.5 . .
C13 C14 C15 119.0(7) . .
C13 C14 H14 120.5 . .
C15 C14 H14 120.5 . .
C16 C15 C14 120.5(7) . .
C16 C15 H15 119.8 . .
C14 C15 H15 119.8 . .
C15 C16 C11 120.5(6) . .
C15 C16 H16 119.7 . .
C11 C16 H16 119.7 . .
Cu1 O17 H17 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.046(5) 2
Cu1 N1 2.046(5) 4
Cu1 N1 2.046(5) 3
Cu1 N1 2.046(5) .
Cu1 O17 2.310(9) .
S1 O18 1.478(4) 8_656
S1 O18 1.478(4) 7_666
S1 O18 1.478(4) 2_655
S1 O18 1.478(4) .
N1 C2 1.334(8) .
N1 C6 1.351(8) .
C2 C3 1.390(8) .
C2 H2 0.9300 .
C3 C4 1.382(9) .
C3 N7 1.415(8) .
C4 C5 1.369(9) .
C4 H4 0.9300 .
C5 C6 1.380(8) .
C5 H5 0.9300 .
C6 H6 0.9300 .
N7 C8 1.348(9) .
N7 H7 0.8600 .
C8 O9 1.240(8) .
C8 N10 1.360(8) .
N10 C11 1.410(9) .
N10 H10 0.8600 .
C11 C12 1.384(9) .
C11 C16 1.405(9) .
C12 C13 1.373(11) .
C12 H12 0.9300 .
C13 C14 1.384(10) .
C13 H13 0.9300 .
C14 C15 1.389(10) .
C14 H14 0.9300 .
C15 C16 1.360(10) .
C15 H15 0.9300 .
C16 H16 0.9300 .
O17 H17 0.8200 .
O19A O19B 1.22(3) .
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
N10 H10 O18 0.86 1.98 2.827(7) 168.3 3
N7 H7 O18 0.86 2.19 2.982(6) 152.8 5_666
