#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/52/04/1520435.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_1520435
loop_
_publ_author_name
'Cheetham, A.K.'
'Bennett, T.D.'
'Callear, Samantha K.'
'Hursthouse, Michael B.'
_publ_section_title
;
 C7.5H9.5N4.5O0.5Zn
;
_journal_name_full               'Crystal Structure Report Archive'
_journal_page_first              625
_journal_year                    2009
_chemical_formula_sum            'C7.5 H9.5 N4.5 O0.5 Zn'
_chemical_formula_weight         236.07
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   15.5741(6)
_cell_length_b                   14.8047(4)
_cell_length_c                   18.4602(8)
_cell_measurement_reflns_used    29517
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     4256.4(3)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31399
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    2.277
_exptl_absorpt_correction_T_max  0.8043
_exptl_absorpt_correction_T_min  0.4783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4866
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0479P)²+2.6300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                3217
_reflns_number_total             4866
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            eCrystal-625.cif
_cod_data_source_block           2009src0013pbca
_cod_depositor_comments
;
Citation :
Cheetham, A.K. and Bennett, T.D. and Callear, Samantha K. and 
Hursthouse, Michael B. (2009) 
University of Southampton, Crystal Structure Report Archive. 
(doi:10.5258/ecrystals/625)

More at:
http://ecrystals.chem.soton.ac.uk/625/
;
_cod_original_sg_symbol_H-M      Pbca
_cod_original_formula_sum        'C7.50 H9.50 N4.50 O0.50 Zn'
_cod_database_code               1520435
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-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
_atom_site_disorder_assembly
_atom_site_disorder_group
C52 C 0.2689(4) 1.1611(4) 0.6069(4) 0.0459(17) Uiso 0.791(8) 1 d PD A 1
H52 H 0.2906 1.1892 0.6494 0.055 Uiso 0.791(8) 1 calc PR A 1
C54 C 0.1482(4) 1.1365(4) 0.5270(4) 0.059(2) Uiso 0.791(8) 1 d PD A 1
H54A H 0.1934 1.1125 0.4955 0.089 Uiso 0.791(8) 1 calc PR A 1
H54B H 0.1195 1.1870 0.5027 0.089 Uiso 0.791(8) 1 calc PR A 1
H54C H 0.1062 1.0889 0.5374 0.089 Uiso 0.791(8) 1 calc PR A 1
C55 C 0.1272(6) 1.2121(6) 0.6434(6) 0.106(3) Uiso 0.791(8) 1 d PD A 1
H55A H 0.1589 1.2286 0.6873 0.158 Uiso 0.791(8) 1 calc PR A 1
H55B H 0.0801 1.1711 0.6562 0.158 Uiso 0.791(8) 1 calc PR A 1
H55C H 0.1037 1.2666 0.6208 0.158 Uiso 0.791(8) 1 calc PR A 1
N53 N 0.1851(4) 1.1670(5) 0.5927(3) 0.048(2) Uiso 0.791(8) 1 d PD A 1
O51 O 0.3203(3) 1.1199(4) 0.5662(4) 0.054(2) Uiso 0.791(8) 1 d PD A 1
C62 C 0.2436(13) 1.1599(17) 0.5460(13) 0.073(9) Uiso 0.209(8) 1 d PD A 2
H62 H 0.2321 1.1490 0.4962 0.087 Uiso 0.209(8) 1 calc PR A 2
C64 C 0.1077(16) 1.239(2) 0.5702(18) 0.106(13) Uiso 0.209(8) 1 d PD A 2
H64A H 0.1162 1.2740 0.5257 0.159 Uiso 0.209(8) 1 calc PR A 2
H64B H 0.0903 1.2796 0.6095 0.159 Uiso 0.209(8) 1 calc PR A 2
H64C H 0.0627 1.1938 0.5622 0.159 Uiso 0.209(8) 1 calc PR A 2
C65 C 0.204(2) 1.199(3) 0.6678(13) 0.128(15) Uiso 0.209(8) 1 d PD A 2
H65A H 0.1564 1.1718 0.6948 0.192 Uiso 0.209(8) 1 calc PR A 2
H65B H 0.2104 1.2625 0.6827 0.192 Uiso 0.209(8) 1 calc PR A 2
H65C H 0.2571 1.1664 0.6778 0.192 Uiso 0.209(8) 1 calc PR A 2
N63 N 0.1850(10) 1.1954(15) 0.5891(9) 0.029(5) Uiso 0.209(8) 1 d PD A 2
O61 O 0.3161(11) 1.1411(14) 0.5737(12) 0.036(6) Uiso 0.209(8) 1 d PD A 2
C2 C 0.1047(2) 0.8445(2) 0.5519(2) 0.0243(8) Uani 1 1 d . . .
H2 H 0.0615 0.8108 0.5275 0.029 Uiso 1 1 calc R . .
C4 C 0.2203(3) 0.9171(3) 0.5733(2) 0.0464(12) Uani 1 1 d . . .
H4 H 0.2747 0.9454 0.5683 0.056 Uiso 1 1 calc R . .
C5 C 0.1744(3) 0.9117(3) 0.6352(2) 0.0462(12) Uani 1 1 d . . .
H5 H 0.1909 0.9362 0.6807 0.055 Uiso 1 1 calc R . .
N1 N 0.10039(18) 0.8651(2) 0.62171(17) 0.0255(7) Uani 1 1 d . . .
N3 N 0.17545(19) 0.8753(2) 0.51892(17) 0.0268(7) Uani 1 1 d . . .
C22 C 0.0975(2) 0.7362(2) 0.8076(2) 0.0269(9) Uani 1 1 d . . .
H22 H 0.0991 0.6834 0.7785 0.032 Uiso 1 1 calc R . .
C24 C 0.0713(3) 0.6292(3) 0.3444(2) 0.0342(10) Uani 1 1 d . . .
H24 H 0.0512 0.5687 0.3470 0.041 Uiso 1 1 calc R . .
C25 C 0.1166(3) 0.6721(3) 0.3961(2) 0.0345(10) Uani 1 1 d . . .
H25 H 0.1338 0.6466 0.4410 0.041 Uiso 1 1 calc R . .
N21 N 0.13403(18) 0.7585(2) 0.37369(17) 0.0268(7) Uani 1 1 d . . .
N23 N 0.05890(19) 0.8126(2) 0.78730(17) 0.0273(7) Uani 1 1 d . . .
C32 C -0.1432(2) 0.7321(3) 0.6412(2) 0.0285(9) Uani 1 1 d . . .
H32 H -0.1790 0.7776 0.6615 0.034 Uiso 1 1 calc R . .
C34 C -0.0311(2) 0.6562(3) 0.6110(2) 0.0339(10) Uani 1 1 d . . .
H34 H 0.0266 0.6364 0.6057 0.041 Uiso 1 1 calc R . .
N31 N 0.32637(19) 0.8378(2) 0.39611(17) 0.0276(7) Uani 1 1 d . . .
N33 N -0.05757(18) 0.7325(2) 0.64752(17) 0.0268(7) Uani 1 1 d . . .
C42 C -0.0943(2) 0.9878(2) 0.6379(2) 0.0258(8) Uani 1 1 d . . .
H42 H -0.0587 0.9905 0.5961 0.031 Uiso 1 1 calc R . .
C43 C 0.3988(2) 0.8858(3) 0.4159(2) 0.0347(10) Uani 1 1 d . . .
H43 H 0.3992 0.9396 0.4440 0.042 Uiso 1 1 calc R . .
C44 C 0.1970(3) 0.9871(3) 0.2880(2) 0.0402(11) Uani 1 1 d . . .
H44 H 0.2479 0.9641 0.2664 0.048 Uiso 1 1 calc R . .
C45 C -0.1427(3) 0.9517(3) 0.7424(2) 0.0393(10) Uani 1 1 d . . .
H45 H -0.1493 0.9249 0.7888 0.047 Uiso 1 1 calc R . .
N41 N -0.07706(19) 0.9353(2) 0.69482(16) 0.0264(7) Uani 1 1 d . . .
N43 N 0.16610(19) 0.9640(2) 0.35509(18) 0.0286(7) Uani 1 1 d . . .
Zn1 Zn 0.20321(3) 0.85916(3) 0.41570(2) 0.02432(14) Uani 1 1 d . . .
Zn2 Zn 0.00771(3) 0.83445(3) 0.69134(2) 0.02552(14) Uani 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'
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
O51 C52 N53 122.5(7) . .
O51 C52 H52 118.7 . .
N53 C52 H52 118.7 . .
C52 N53 C54 123.0(6) . .
C52 N53 C55 120.5(7) . .
C54 N53 C55 116.4(6) . .
O61 C62 N63 117(2) . .
O61 C62 H62 121.3 . .
N63 C62 H62 121.3 . .
N63 C64 H64A 109.5 . .
N63 C64 H64B 109.5 . .
H64A C64 H64B 109.5 . .
N63 C64 H64C 109.5 . .
H64A C64 H64C 109.5 . .
H64B C64 H64C 109.5 . .
N63 C65 H65A 109.5 . .
N63 C65 H65B 109.5 . .
H65A C65 H65B 109.5 . .
N63 C65 H65C 109.5 . .
H65A C65 H65C 109.5 . .
H65B C65 H65C 109.5 . .
C62 N63 C64 128.6(19) . .
C62 N63 C65 118.0(18) . .
C64 N63 C65 113.1(19) . .
N1 C2 N3 113.9(3) . .
N1 C2 H2 123.1 . .
N3 C2 H2 123.1 . .
C5 C4 N3 108.9(4) . .
C5 C4 H4 125.6 . .
N3 C4 H4 125.6 . .
C4 C5 N1 108.8(4) . .
C4 C5 H5 125.6 . .
N1 C5 H5 125.6 . .
C2 N1 C5 104.5(3) . .
C2 N1 Zn2 127.8(2) . .
C5 N1 Zn2 127.6(3) . .
C2 N3 C4 103.9(3) . .
C2 N3 Zn1 125.4(2) . .
C4 N3 Zn1 130.7(3) . .
N23 C22 N21 113.3(3) . 7_576
N23 C22 H22 123.4 . .
N21 C22 H22 123.4 7_576 .
C25 C24 N23 108.7(3) . 7_575
C25 C24 H24 125.7 . .
N23 C24 H24 125.7 7_575 .
C24 C25 N21 109.3(4) . .
C24 C25 H25 125.3 . .
N21 C25 H25 125.3 . .
C22 N21 C25 104.1(3) 7_575 .
C22 N21 Zn1 122.4(2) 7_575 .
C25 N21 Zn1 133.3(3) . .
C22 N23 C24 104.6(3) . 7_576
C22 N23 Zn2 125.1(3) . .
C24 N23 Zn2 130.0(3) 7_576 .
N31 C32 N33 113.8(3) 4_466 .
N31 C32 H32 123.1 4_466 .
N33 C32 H32 123.1 . .
C43 C34 N33 108.3(3) 4_466 .
C43 C34 H34 125.8 4_466 .
N33 C34 H34 125.8 . .
C32 N31 C43 104.3(3) 4_566 .
C32 N31 Zn1 124.3(3) 4_566 .
C43 N31 Zn1 131.4(3) . .
C32 N33 C34 104.6(3) . .
C32 N33 Zn2 123.2(3) . .
C34 N33 Zn2 131.8(2) . .
N43 C42 N41 113.8(3) 5_576 .
N43 C42 H42 123.1 5_576 .
N41 C42 H42 123.1 . .
C34 C43 N31 109.0(4) 4_566 .
C34 C43 H43 125.5 4_566 .
N31 C43 H43 125.5 . .
C45 C44 N43 108.6(3) 5_576 .
C45 C44 H44 125.7 5_576 .
N43 C44 H44 125.7 . .
C44 C45 N41 108.5(4) 5_576 .
C44 C45 H45 125.7 5_576 .
N41 C45 H45 125.7 . .
C42 N41 C45 104.5(3) . .
C42 N41 Zn2 122.9(3) . .
C45 N41 Zn2 130.4(3) . .
C42 N43 C44 104.5(3) 5_576 .
C42 N43 Zn1 127.1(3) 5_576 .
C44 N43 Zn1 126.6(3) . .
N3 Zn1 N31 114.17(13) . .
N3 Zn1 N21 110.38(12) . .
N31 Zn1 N21 109.48(13) . .
N3 Zn1 N43 112.59(13) . .
N31 Zn1 N43 107.58(12) . .
N21 Zn1 N43 101.90(13) . .
N23 Zn2 N1 109.00(12) . .
N23 Zn2 N33 116.60(13) . .
N1 Zn2 N33 106.35(12) . .
N23 Zn2 N41 111.23(13) . .
N1 Zn2 N41 109.32(12) . .
N33 Zn2 N41 104.02(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C52 O51 1.256(8) .
C52 N53 1.334(8) .
C52 H52 0.9500 .
C54 N53 1.416(8) .
C54 H54A 0.9800 .
C54 H54B 0.9800 .
C54 H54C 0.9800 .
C55 N53 1.461(10) .
C55 H55A 0.9800 .
C55 H55B 0.9800 .
C55 H55C 0.9800 .
C62 O61 1.270(18) .
C62 N63 1.320(17) .
C62 H62 0.9500 .
C64 N63 1.411(17) .
C64 H64A 0.9800 .
C64 H64B 0.9800 .
C64 H64C 0.9800 .
C65 N63 1.482(18) .
C65 H65A 0.9800 .
C65 H65B 0.9800 .
C65 H65C 0.9800 .
C2 N1 1.326(5) .
C2 N3 1.339(4) .
C2 H2 0.9500 .
C4 C5 1.350(6) .
C4 N3 1.371(5) .
C4 H4 0.9500 .
C5 N1 1.366(5) .
C5 H5 0.9500 .
N1 Zn2 1.986(3) .
N3 Zn1 1.968(3) .
C22 N23 1.335(5) .
C22 N21 1.348(5) 7_576
C22 H22 0.9500 .
C24 C25 1.346(5) .
C24 N23 1.376(5) 7_575
C24 H24 0.9500 .
C25 N21 1.371(5) .
C25 H25 0.9500 .
N21 C22 1.348(5) 7_575
N21 Zn1 1.995(3) .
N23 C24 1.376(5) 7_576
N23 Zn2 1.969(3) .
C32 N31 1.331(5) 4_466
C32 N33 1.339(4) .
C32 H32 0.9500 .
C34 C43 1.352(5) 4_466
C34 N33 1.379(5) .
C34 H34 0.9500 .
N31 C32 1.331(5) 4_566
N31 C43 1.382(5) .
N31 Zn1 1.977(3) .
N33 Zn2 1.991(3) .
C42 N43 1.333(4) 5_576
C42 N41 1.335(5) .
C42 H42 0.9500 .
C43 C34 1.352(5) 4_566
C43 H43 0.9500 .
C44 C45 1.361(6) 5_576
C44 N43 1.372(5) .
C44 H44 0.9500 .
C45 C44 1.361(6) 5_576
C45 N41 1.370(5) .
C45 H45 0.9500 .
N41 Zn2 1.994(3) .
N43 C42 1.333(4) 5_576
N43 Zn1 1.999(3) .
