#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/56/2005646.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2005646
loop_
_publ_author_name
'Price, C. L.'
'Taylor, M. R.'
_publ_contact_author
;
   Dr Max R. Taylor
   Department of Chemistry
   The Flinders University of South Australia
   GPO Box 2100
   Adelaide 5001
   Australia
;
_publ_section_title
;
 7-Methyl-3-adeninium Trichloro(7-methyladenine-N⁹)zinc(II)
 Hydrate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2736
_journal_page_last               2738
_journal_paper_doi               10.1107/S0108270196009079
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '(C6 H8 N5) [Zn Cl3 (C6 H7 N5)] , H2 O'
_chemical_formula_moiety         'C6 H8 N5 1+, C6 H7 Cl3 N5 Zn 1-, H2 O'
_chemical_formula_structural     '(C6 H8 N5)((C6 H7 N5) Zn Cl3)(H2 O)'
_chemical_formula_sum            'C12 H17 Cl3 N10 O Zn'
_chemical_formula_weight         488.94
_chemical_name_systematic
;
 7-methyladeninium trichloro-7-methyladeninezinc(II) hydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90.00000
_cell_angle_beta                 97.378(5)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   7.214(1)
_cell_length_b                   16.437(1)
_cell_length_c                   16.180(2)
_cell_measurement_reflns_used    11
_cell_measurement_temperature    293
_cell_measurement_theta_max      31.97
_cell_measurement_theta_min      30.01
_cell_volume                     1902.7(4)
_computing_data_reduction
Xtal3.2_DIFDAT_ADDREF_ABSORB_SORTRF_(Hall,_Flack_&_Stewart,_1992)
_computing_molecular_graphics    Xtal3.2
_computing_publication_material  Xtal3.2_BONDLA_CIFIO
_computing_structure_refinement  Xtal3.2_CRYLSQ
_computing_structure_solution    Xtal3.2
_diffrn_ambient_temperature      293
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'ω/2θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  .012
_diffrn_reflns_av_sigmaI/netI    .019
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            3728
_diffrn_reflns_theta_max         69.92
_diffrn_reflns_theta_min         3.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    5.91
_exptl_absorpt_correction_T_max  .4306
_exptl_absorpt_correction_T_min  .1881
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_meas      1.71(1)
_exptl_crystal_density_method
;
 flotation in 1,1,1-trichloroethane and 1,2-dibromoethane
;
_exptl_crystal_description       prism
_exptl_crystal_F_000             991.69
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.186
_refine_diff_density_max         .444
_refine_diff_density_min         -.366
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.903
_refine_ls_goodness_of_fit_obs   2.959
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     312
_refine_ls_number_reflns         3599
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .035
_refine_ls_R_factor_obs          .032
_refine_ls_shift/esd_max
'1.921 for U~iso~ of H111', 0.31 for non-H atoms'
_refine_ls_shift/esd_mean        .126
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .07
_refine_ls_wR_factor_obs         .07
_reflns_number_observed          3451
_reflns_number_total             3599
_reflns_observed_criterion       refl_observed_if_Fsqd_>_0
_cod_data_source_file            kh1103.cif
_cod_data_source_block           znade
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C12 H17 Cl3 N10 O1 Zn1'
_cod_database_code               2005646
_cod_database_fobs_code          2005646
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,1/2+y,1/2-z
-x,-y,-z
+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
Zn .65067(4) .58631(2) .33875(2) .0289(1) Uani
Cl1 .7101(1) .46601(4) .40409(5) .0570(4) Uani
Cl2 .86876(8) .61127(4) .25470(4) .0382(3) Uani
Cl3 .36621(9) .59079(4) .26173(4) .0476(3) Uani
N1 .5606(3) .9132(1) .4343(1) .036(1) Uani
C2 .5913(4) .8756(2) .3639(2) .039(1) Uani
N3 .6234(3) .7974(1) .3513(1) .036(1) Uani
C4 .6258(3) .7540(1) .4218(1) .029(1) Uani
C5 .6001(3) .7858(1) .4989(1) .027(1) Uani
C6 .5639(3) .8698(1) .5049(1) .030(1) Uani
N7 .6114(3) .7200(1) .5536(1) .0295(9) Uani
C8 .6420(3) .6543(1) .5088(1) .032(1) Uani
N9 .6512(3) .6708(1) .4294(1) .0314(9) Uani
C10 .5922(5) .7194(2) .6428(2) .041(1) Uani
N11 .5285(4) .9081(1) .5737(1) .044(1) Uani
N1' .1129(3) .7506(1) .5476(1) .038(1) Uani
C2' .0732(4) .8202(2) .5807(2) .039(1) Uani
N3' .0448(3) .8905(1) .5406(1) .034(1) Uani
C4' .0635(3) .8905(1) .4583(1) .030(1) Uani
C5' .1046(3) .8195(1) .4186(1) .028(1) Uani
C6' .1282(3) .7465(1) .4648(1) .030(1) Uani
N7' .1137(3) .8432(1) .3371(1) .0316(9) Uani
C8' .0790(4) .9231(2) .3340(2) .040(1) Uani
N9' .0480(3) .9550(1) .4063(1) .039(1) Uani
C10' .1474(5) .7932(2) .2659(2) .043(1) Uani
N11' .1683(4) .6742(1) .4359(1) .041(1) Uani
O .1403(5) .4508(2) .3548(2) .088(2) Uani
H110 .603(5) .670(2) .661(2) .07(1) Uiso
H210 .476(5) .736(2) .652(2) .06(1) Uiso
H310 .674(5) .755(2) .668(2) .06(1) Uiso
H111 .537(5) .884(2) .616(2) .05(1) Uiso
H211 .507(4) .959(2) .570(2) .047(9) Uiso
H2 .582(4) .909(2) .312(2) .049(8) Uiso
H8 .660(4) .604(2) .529(2) .040(7) Uiso
H110' .143(5) .825(2) .220(2) .08(1) Uiso
H210' .272(5) .758(2) .278(2) .07(1) Uiso
H310' .050(5) .749(2) .257(2) .09(1) Uiso
H111' .188(5) .666(2) .391(2) .04(1) Uiso
H211' .184(4) .632(2) .472(2) .050(9) Uiso
H2' .052(4) .821(2) .636(2) .050(8) Uiso
H3' .015(5) .930(2) .566(2) .06(1) Uiso
H8' .082(4) .950(2) .285(2) .052(9) Uiso
H1'' .036(9) .464(4) .384(4) .19(3) Uiso
H2'' .18(1) .497(7) .334(6) .32(6) Uiso
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn -1.612 .678 IntTabIV_Tables_2.2B_and_2.3.1
Cl .348 .702 IntTabIV_Tables_2.2B_and_2.3.1
C .017 .009 IntTabIV_Tables_2.2B_and_2.3.1
N .029 .018 IntTabIV_Tables_2.2B_and_2.3.1
H 0 0 IntTabIV_Tables_2.2B_and_2.3.1
O .047 .032 IntTabIV_Tables_2.2B_and_2.3.1
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
4 5 3
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3' H3' N9' 1_555 1_576 1_576 72.4(7) ?
N3' H3' N9' 2_555 2_576 2_576 123.7(8) ?
N3' H3' N9' 3_555 3_576 3_576 107.2(8) ?
N3' H3' N9' 4_555 4_576 4_576 54.1(7) ?
N1 H211 N11 3_555 3_564 3_564 132(2) ?
Cl1 Zn Cl2 . . . 109.75(3) yes
Cl1 Zn Cl3 . . . 113.02(3) yes
Cl1 Zn N9 . . . 106.22(6) yes
Cl2 Zn Cl3 . . . 108.49(3) yes
Cl2 Zn N9 . . . 112.24(6) yes
Cl3 Zn N9 . . . 107.15(6) yes
C2 N1 C6 . . . 119.5(2) yes
N1 C2 N3 . . . 129.0(2) yes
N1 C2 H2 . . . 117(2) ?
N3 C2 H2 . . . 114(2) ?
C2 N3 C4 . . . 111.6(2) yes
N3 C4 C5 . . . 125.1(2) yes
N3 C4 N9 . . . 126.1(2) yes
C5 C4 N9 . . . 108.8(2) yes
C4 C5 C6 . . . 118.5(2) yes
C4 C5 N7 . . . 106.0(2) yes
C6 C5 N7 . . . 135.4(2) yes
N1 C6 C5 . . . 116.3(2) yes
N1 C6 N11 . . . 118.4(2) yes
C5 C6 N11 . . . 125.2(2) yes
C5 N7 C8 . . . 106.5(2) yes
C5 N7 C10 . . . 128.6(2) yes
C8 N7 C10 . . . 124.8(2) yes
N7 C8 N9 . . . 113.1(2) yes
N7 C8 H8 . . . 125(2) ?
N9 C8 H8 . . . 121(2) ?
Zn N9 C4 . . . 128.80(10) yes
Zn N9 C8 . . . 124.70(10) yes
C4 N9 C8 . . . 105.5(2) yes
N7 C10 H110 . . . 109(2) ?
N7 C10 H210 . . . 111(2) ?
N7 C10 H310 . . . 107(2) ?
H110 C10 H210 . . . 106(3) ?
H110 C10 H310 . . . 116(3) ?
H210 C10 H310 . . . 107(3) ?
C6 N11 H111 . . . 120(3) ?
C6 N11 H211 . . . 117(2) ?
H111 N11 H211 . . . 123(3) ?
C2' N1' C6' . . . 119.7(2) yes
N1' C2' N3' . . . 126.0(2) yes
N1' C2' H2' . . . 118(2) ?
N3' C2' H2' . . . 116(2) ?
C2' N3' C4' . . . 116.8(2) yes
C2' N3' H3' . . . 119(2) ?
C4' N3' H3' . . . 124(2) ?
N3' C4' C5' . . . 120.8(2) yes
N3' C4' N9' . . . 126.9(2) yes
C5' C4' N9' . . . 112.3(2) yes
C4' C5' C6' . . . 119.3(2) yes
C4' C5' N7' . . . 104.1(2) yes
C6' C5' N7' . . . 136.6(2) yes
N1' C6' C5' . . . 117.4(2) yes
N1' C6' N11' . . . 116.3(2) yes
C5' C6' N11' . . . 126.3(2) yes
C5' N7' C8' . . . 106.3(2) yes
C5' N7' C10' . . . 128.8(2) yes
C8' N7' C10' . . . 124.9(2) yes
N7' C8' N9' . . . 114.0(2) yes
N7' C8' H8' . . . 119(2) ?
N9' C8' H8' . . . 127(2) ?
C4' N9' C8' . . . 103.3(2) yes
N7' C10' H110' . . . 109(2) ?
N7' C10' H210' . . . 112(2) ?
N7' C10' H310' . . . 109(2) ?
H110' C10' H210' . . . 114(3) ?
H110' C10' H310' . . . 110(3) ?
H210' C10' H310' . . . 101(3) ?
C6' N11' H111' . . . 124(2) ?
C6' N11' H211' . . . 118(2) ?
H111' N11' H211' . . . 117(3) ?
H1'' O H2'' . . . 108(8) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Zn Cl1 2.2572(8) yes
Zn Cl2 2.2456(8) yes
Zn Cl3 2.2612(7) yes
Zn N9 2.020(2) yes
N1 C2 1.339(3) yes
N1 C6 1.344(3) yes
C2 N3 1.326(3) yes
C2 H2 1.00(3) ?
N3 C4 1.342(3) yes
C4 C5 1.387(3) yes
C4 N9 1.384(3) yes
C5 C6 1.412(3) yes
C5 N7 1.392(3) yes
C6 N11 1.332(3) yes
N7 C8 1.335(3) yes
N7 C10 1.467(3) yes
C8 N9 1.322(3) yes
C8 H8 .89(3) ?
C10 H110 .86(4) ?
C10 H210 .91(3) ?
C10 H310 .89(3) ?
N11 H111 .78(3) ?
N11 H211 .84(3) ?
N1' C2' 1.311(3) yes
N1' C6' 1.360(3) yes
C2' N3' 1.328(3) yes
C2' H2' .93(3) ?
N3' C4' 1.356(3) yes
N3' H3' .82(3) ?
C4' C5' 1.383(3) yes
C4' N9' 1.350(3) yes
C5' C6' 1.413(3) yes
C5' N7' 1.385(3) yes
C6' N11' 1.323(3) yes
N7' C8' 1.337(3) yes
N7' C10' 1.460(3) yes
C8' N9' 1.326(3) yes
C8' H8' .90(3) ?
C10' H110' .91(4) ?
C10' H210' 1.06(3) ?
C10' H310' 1.01(4) ?
N11' H111' .77(4) ?
N11' H211' .91(3) ?
O H1'' .96(7) ?
O H2'' .90(10) ?
