#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:34:52 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180511 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/80/7218030.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_7218030
loop_
_publ_author_name
'De la Pinta, Noelia'
'Caballero, Ana B.'
'Madariaga, Gotzon'
'Ezpeleta, José M.'
'Rodriguez-Dieguez, Antonio'
'Salas, Juan M.'
'Cortés, Roberto'
_publ_section_title
;
 DPDS--DPS in situ transformation at room temperature via a
 1,2-nucleophilic addition mechanism
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              8322
_journal_paper_doi               10.1039/C4CE00781F
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C40 H38 Cl2 N8 O11 S4 Zn'
_chemical_formula_weight         1071.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 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            4
_cell_length_a                   16.529(2)
_cell_length_b                   16.529(2)
_cell_length_c                   16.604(2)
_cell_measurement_temperature    293(2)
_cell_volume                     4536.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28832
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.0021
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.002
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.026(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0460
_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)+(0.0707P)²+3.2047P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1195
_reflns_number_gt                4875
_reflns_number_total             5315
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7216463
_cod_data_source_file            c4ce00781f2.cif
_cod_data_source_block           an232
_cod_original_cell_volume        4536.3(11)
_cod_original_sg_symbol_H-M      P41212
_cod_database_code               7218030
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'-y, -x, -z+1/2'
'y, x, -z'
'y+1/2, -x+1/2, z+3/4'
'-y+1/2, x+1/2, z+1/4'
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
Zn1 Zn 0.005164(19) 1.005164(19) 0.5000 0.02195(12) Uani 1 2 d S
S2 S -0.00233(6) 0.60227(5) 0.46181(6) 0.0381(2) Uani 1 1 d .
S1 S 0.07535(6) 1.40411(5) 0.53448(7) 0.0386(2) Uani 1 1 d .
Cl1 Cl 0.19625(5) 1.22252(5) 0.22747(5) 0.0360(2) Uani 1 1 d .
O5 O 0.05611(15) 0.94389(15) 0.2500 0.0378(8) Uani 1 2 d S
N1 N 0.01281(16) 1.13453(15) 0.52581(16) 0.0249(5) Uani 1 1 d .
N2 N 0.00601(15) 0.87642(15) 0.48762(14) 0.0229(5) Uani 1 1 d .
N4 N 0.33092(17) 1.41948(17) 0.42795(16) 0.0289(6) Uani 1 1 d .
O1W O -0.01499(15) 1.03107(15) 0.37456(13) 0.0276(5) Uani 1 1 d .
C6 C 0.05129(19) 0.7545(2) 0.4248(2) 0.0282(6) Uani 1 1 d .
H6 H 0.0842 0.7295 0.3868 0.034 Uiso 1 1 calc R
C7 C 0.0002(2) 0.70891(18) 0.4735(2) 0.0283(6) Uani 1 1 d .
C8 C -0.04194(19) 0.83174(19) 0.53599(19) 0.0250(6) Uani 1 1 d .
H8 H -0.0736 0.8580 0.5742 0.030 Uiso 1 1 calc R
C9 C 0.1748(2) 1.4055(2) 0.4935(2) 0.0297(7) Uani 1 1 d .
C10 C 0.05245(19) 0.8372(2) 0.43390(19) 0.0264(6) Uani 1 1 d .
H10 H 0.0869 0.8674 0.4014 0.032 Uiso 1 1 calc R
C11 C 0.0755(2) 1.1623(2) 0.5701(2) 0.0278(7) Uani 1 1 d .
H11 H 0.1055 1.1253 0.5999 0.033 Uiso 1 1 calc R
C12 C 0.0974(2) 1.2439(2) 0.5734(2) 0.0303(7) Uani 1 1 d .
H12 H 0.1418 1.2606 0.6036 0.036 Uiso 1 1 calc R
O1 O 0.28106(18) 1.2247(3) 0.2451(2) 0.0684(10) Uani 1 1 d .
N3 N -0.2750(2) 0.5540(2) 0.4648(2) 0.0457(8) Uani 1 1 d .
O4 O 0.17592(19) 1.1529(2) 0.1821(2) 0.0664(10) Uani 1 1 d .
C16 C 0.2033(2) 1.3498(2) 0.4386(2) 0.0328(7) Uani 1 1 d .
H16 H 0.1709 1.3068 0.4225 0.039 Uiso 1 1 calc R
C17 C -0.0459(2) 0.7481(2) 0.5308(2) 0.0289(7) Uani 1 1 d .
H17 H -0.0790 0.7188 0.5655 0.035 Uiso 1 1 calc R
C18 C -0.0155(2) 1.2725(2) 0.4887(2) 0.0329(7) Uani 1 1 d .
H18 H -0.0489 1.3090 0.4621 0.039 Uiso 1 1 calc R
C19 C 0.2802(2) 1.3584(2) 0.4080(2) 0.0329(7) Uani 1 1 d .
H19 H 0.2984 1.3200 0.3714 0.039 Uiso 1 1 calc R
C20 C 0.0517(2) 1.29920(19) 0.5308(2) 0.0305(7) Uani 1 1 d .
C21 C -0.0320(2) 1.1898(2) 0.4872(2) 0.0299(7) Uani 1 1 d .
H21 H -0.0765 1.1721 0.4578 0.036 Uiso 1 1 calc R
C22 C -0.1085(2) 0.5850(2) 0.4616(2) 0.0337(7) Uani 1 1 d .
O3 O 0.1542(2) 1.2156(3) 0.3033(2) 0.0689(10) Uani 1 1 d .
C24 C 0.3018(2) 1.4740(2) 0.4804(2) 0.0351(8) Uani 1 1 d .
H24 H 0.3349 1.5171 0.4947 0.042 Uiso 1 1 calc R
C25 C 0.2249(2) 1.4697(2) 0.5148(2) 0.0316(7) Uani 1 1 d .
H25 H 0.2075 1.5089 0.5511 0.038 Uiso 1 1 calc R
C26 C -0.2206(3) 0.4995(2) 0.4906(2) 0.0463(10) Uani 1 1 d .
H26 H -0.2398 0.4504 0.5103 0.056 Uiso 1 1 calc R
C27 C -0.1383(2) 0.5118(2) 0.4899(2) 0.0390(8) Uani 1 1 d .
H27 H -0.1032 0.4718 0.5080 0.047 Uiso 1 1 calc R
C28 C -0.1641(2) 0.6409(2) 0.4315(2) 0.0387(8) Uani 1 1 d .
H28 H -0.1466 0.6895 0.4092 0.046 Uiso 1 1 calc R
C29 C -0.2457(2) 0.6228(2) 0.4355(2) 0.0389(8) Uani 1 1 d .
H29 H -0.2823 0.6611 0.4166 0.047 Uiso 1 1 calc R
O2 O 0.1669(3) 1.2925(2) 0.1888(3) 0.1008(17) Uani 1 1 d .
H12W H 0.007(2) 1.001(3) 0.346(3) 0.037(11) Uiso 1 1 d .
H11W H -0.058(3) 1.049(3) 0.364(3) 0.058(15) Uiso 1 1 d .
H51 H 0.111(2) 0.947(2) 0.263(2) 0.039(11) 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
N2 Zn1 N2 91.27(14) 6_466 .
N2 Zn1 O1W 86.43(9) 6_466 .
N2 Zn1 O1W 96.08(9) . .
N2 Zn1 O1W 96.08(9) 6_466 6_466
N2 Zn1 O1W 86.43(9) . 6_466
O1W Zn1 O1W 176.42(13) . 6_466
N2 Zn1 N1 91.85(9) 6_466 .
N2 Zn1 N1 173.11(10) . .
O1W Zn1 N1 90.24(10) . .
O1W Zn1 N1 87.14(10) 6_466 .
N2 Zn1 N1 173.11(10) 6_466 6_466
N2 Zn1 N1 91.85(9) . 6_466
O1W Zn1 N1 87.14(10) . 6_466
O1W Zn1 N1 90.24(10) 6_466 6_466
N1 Zn1 N1 85.71(14) . 6_466
C7 S2 C22 100.52(17) . .
C20 S1 C9 101.65(16) . .
O2 Cl1 O4 110.1(2) . .
O2 Cl1 O1 114.2(3) . .
O4 Cl1 O1 111.2(2) . .
O2 Cl1 O3 107.3(3) . .
O4 Cl1 O3 106.6(2) . .
O1 Cl1 O3 107.1(2) . .
C21 N1 C11 116.9(3) . .
C21 N1 Zn1 122.8(2) . .
C11 N1 Zn1 118.9(2) . .
C10 N2 C8 117.9(3) . .
C10 N2 Zn1 123.2(2) . .
C8 N2 Zn1 118.9(2) . .
C24 N4 C19 115.9(3) . .
C10 C6 C7 118.9(3) . .
C17 C7 C6 118.8(3) . .
C17 C7 S2 121.9(3) . .
C6 C7 S2 119.3(3) . .
N2 C8 C17 122.5(3) . .
C16 C9 C25 118.3(3) . .
C16 C9 S1 124.1(3) . .
C25 C9 S1 117.5(3) . .
N2 C10 C6 123.0(3) . .
N1 C11 C12 123.2(3) . .
C20 C12 C11 118.5(3) . .
C29 N3 C26 116.5(4) . .
C19 C16 C9 119.4(3) . .
C7 C17 C8 119.0(3) . .
C20 C18 C21 118.7(3) . .
N4 C19 C16 124.0(3) . .
C12 C20 C18 119.1(3) . .
C12 C20 S1 120.5(3) . .
C18 C20 S1 120.3(3) . .
N1 C21 C18 123.5(3) . .
C27 C22 C28 117.7(4) . .
C27 C22 S2 119.3(3) . .
C28 C22 S2 123.0(3) . .
N4 C24 C25 124.0(3) . .
C9 C25 C24 118.4(3) . .
N3 C26 C27 124.0(4) . .
C26 C27 C22 118.9(4) . .
C29 C28 C22 118.7(4) . .
N3 C29 C28 124.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N2 2.138(2) 6_466
Zn1 N2 2.138(2) .
Zn1 O1W 2.152(2) .
Zn1 O1W 2.152(2) 6_466
Zn1 N1 2.184(2) .
Zn1 N1 2.184(3) 6_466
S2 C7 1.774(3) .
S2 C22 1.779(4) .
S1 C20 1.779(3) .
S1 C9 1.779(3) .
Cl1 O2 1.408(4) .
Cl1 O4 1.416(3) .
Cl1 O1 1.433(3) .
Cl1 O3 1.443(3) .
N1 C21 1.340(4) .
N1 C11 1.351(4) .
N2 C10 1.343(4) .
N2 C8 1.349(4) .
N4 C24 1.342(4) .
N4 C19 1.353(4) .
C6 C10 1.376(5) .
C6 C7 1.391(5) .
C7 C17 1.380(5) .
C8 C17 1.387(5) .
C9 C16 1.377(5) .
C9 C25 1.393(5) .
C11 C12 1.398(4) .
C12 C20 1.381(5) .
N3 C29 1.328(5) .
N3 C26 1.343(6) .
C16 C19 1.377(5) .
C18 C20 1.384(5) .
C18 C21 1.394(5) .
C22 C27 1.387(5) .
C22 C28 1.396(5) .
C24 C25 1.396(5) .
C26 C27 1.375(6) .
C28 C29 1.384(5) .
