#------------------------------------------------------------------------------
#$Date: 2017-03-05 07:13:48 +0200 (Sun, 05 Mar 2017) $
#$Revision: 193817 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/16/7041681.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_7041681
loop_
_publ_author_name
'Purkait, Suranjana'
'Aullón, Gabriel'
'Zangrando, Ennio'
'Chakraborty, Prateeti'
_publ_section_title
;
 Group 12 metal complexes of
 (2-piperazine-1-yl-ethyl)-pyridin-2-yl-methylene-amine: rare
 participation of terminal piperazine N in coordination leads to
 structural diversity.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2184
_journal_page_last               2195
_journal_paper_doi               10.1039/c6dt04578b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
'C12 H19 Cl2 N4 Zn, C12 H18 Cl7 N4 O Zn2, 2H2O'
_chemical_formula_sum            'C24 H41 Cl7 N8 O2 Zn3'
_chemical_formula_weight         917.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-10 deposited with the CCDC.
2017-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                106.014(5)
_cell_angle_beta                 97.668(5)
_cell_angle_gamma                103.406(5)
_cell_formula_units_Z            1
_cell_length_a                   8.246(5)
_cell_length_b                   8.486(5)
_cell_length_c                   14.876(5)
_cell_measurement_reflns_used    1794
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.36
_cell_measurement_theta_min      2.26
_cell_volume                     951.4(9)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    'Ortep3 for Windows (Farrugia,1997)'
_computing_publication_material  'Wingx 2013.03 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA-PHI 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  0.0400
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9161
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        23.124
_diffrn_reflns_theta_max         23.124
_diffrn_reflns_theta_min         2.546
_exptl_absorpt_coefficient_mu    2.402
_exptl_absorpt_correction_T_max  0.58
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       block
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.276
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0888P)²+1.8625P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1416
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2077
_reflns_number_total             2370
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt04578b2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7041680--7041682.cif.
;
_cod_database_code               7041681
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.44283(7) 0.35014(8) 0.12415(5) 0.0418(3) Uani 1 1 d . . . . .
Zn2 Zn 1.01844(17) 0.66065(18) 0.47335(10) 0.0511(4) Uani 0.5 1 d . . P . .
Cl1 Cl 0.44351(18) 0.16831(18) 0.21021(11) 0.0506(4) Uani 1 1 d . . . . .
Cl2 Cl 0.67447(18) 0.40630(19) 0.06260(11) 0.0507(4) Uani 1 1 d . . . . .
N1 N 0.2680(6) 0.1639(6) -0.0107(3) 0.0443(12) Uani 1 1 d . . . . .
N2 N 0.2214(6) 0.4235(6) 0.1196(4) 0.0442(12) Uani 1 1 d . . . . .
N3 N 0.5201(6) 0.6267(6) 0.2550(3) 0.0448(12) Uani 1 1 d . . . . .
N4 N 0.8185(7) 0.6879(8) 0.4018(4) 0.0646(15) Uani 1 1 d . . . . .
H4A H 0.9039 0.6550 0.4269 0.078 Uiso 1 1 calc R U . . .
H4B H 0.8241 0.7917 0.4393 0.078 Uiso 0.5 1 calc R U P . .
C1 C 0.2949(8) 0.0353(8) -0.0755(4) 0.0463(14) Uani 1 1 d . . . . .
H1 H 0.4016 0.0160 -0.0676 0.056 Uiso 1 1 calc R U . . .
C2 C 0.1698(8) -0.0718(8) -0.1548(5) 0.0537(16) Uani 1 1 d . . . . .
H2 H 0.1921 -0.1616 -0.1988 0.064 Uiso 1 1 calc R U . . .
C3 C 0.0125(8) -0.0424(9) -0.1670(5) 0.0585(17) Uani 1 1 d . . . . .
H3 H -0.0733 -0.1121 -0.2196 0.070 Uiso 1 1 calc R U . . .
C4 C -0.0163(7) 0.0906(8) -0.1008(5) 0.0511(16) Uani 1 1 d . . . . .
H4 H -0.1219 0.1123 -0.1080 0.061 Uiso 1 1 calc R U . . .
C5 C 0.1133(7) 0.1925(8) -0.0229(4) 0.0447(14) Uani 1 1 d . . . . .
C6 C 0.0962(7) 0.3360(8) 0.0503(4) 0.0467(15) Uani 1 1 d . . . . .
H6 H -0.0063 0.3645 0.0469 0.056 Uiso 1 1 calc R U . . .
C7 C 0.2143(8) 0.5729(8) 0.1927(5) 0.0550(17) Uani 1 1 d . . . . .
H7A H 0.1842 0.5426 0.2478 0.066 Uiso 1 1 calc R U . . .
H7B H 0.1287 0.6209 0.1684 0.066 Uiso 1 1 calc R U . . .
C8 C 0.3864(9) 0.7005(8) 0.2207(5) 0.0579(17) Uani 1 1 d . . . . .
H8A H 0.4124 0.7349 0.1660 0.070 Uiso 1 1 calc R U . . .
H8B H 0.3856 0.8012 0.2709 0.070 Uiso 1 1 calc R U . . .
C9 C 0.5080(8) 0.6180(8) 0.3506(4) 0.0535(16) Uani 1 1 d . . . . .
H9A H 0.4014 0.5359 0.3466 0.064 Uiso 1 1 calc R U . . .
H9B H 0.5065 0.7288 0.3910 0.064 Uiso 1 1 calc R U . . .
C10 C 0.6539(8) 0.5670(9) 0.3961(5) 0.0587(17) Uani 1 1 d . . . . .
H10A H 0.6417 0.5657 0.4599 0.070 Uiso 1 1 calc R U . . .
H10B H 0.6514 0.4527 0.3586 0.070 Uiso 1 1 calc R U . . .
C11 C 0.8339(8) 0.6928(10) 0.3046(5) 0.0650(19) Uani 1 1 d . . . . .
H11A H 0.8346 0.5810 0.2650 0.078 Uiso 1 1 calc R U . . .
H11B H 0.9407 0.7741 0.3081 0.078 Uiso 1 1 calc R U . . .
C12 C 0.6888(9) 0.7431(8) 0.2605(5) 0.0608(18) Uani 1 1 d . . . . .
H12A H 0.6941 0.8584 0.2978 0.073 Uiso 1 1 calc R U . . .
H12B H 0.7003 0.7435 0.1965 0.073 Uiso 1 1 calc R U . . .
Cl3 Cl 0.9541(3) 0.6019(3) 0.61357(12) 0.0780(6) Uani 1 1 d . . . . .
Cl4 Cl 1.2304(5) 0.8908(5) 0.4857(4) 0.0930(15) Uani 0.5 1 d . . P . .
O1W O 0.5613(17) 0.8427(17) 0.5880(7) 0.103(4) Uani 0.5 1 d . . P . .
H11W H 0.5436 0.8170 0.6378 0.154 Uiso 0.5 1 d . U P . .
H12W H 0.5844 0.9507 0.6021 0.154 Uiso 0.5 1 d . U P . .
O2W O 0.8341(18) 0.986(3) 0.5282(11) 0.156(9) Uani 0.5 1 d . . P A 2
H21W H 0.9282 0.9962 0.5691 0.235 Uiso 0.5 1 d . U P B 2
H22W H 0.7620 0.8974 0.5358 0.235 Uiso 0.5 1 d . U P C 2
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'
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'
O O 0.0106 0.0060 '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 Cl2 134.75(14) . .
N2 Zn1 N1 75.75(19) . .
Cl2 Zn1 N1 97.01(13) . .
N2 Zn1 Cl1 110.73(14) . .
Cl2 Zn1 Cl1 114.52(6) . .
N1 Zn1 Cl1 97.93(13) . .
N2 Zn1 N3 75.76(18) . .
Cl2 Zn1 N3 96.61(12) . .
N1 Zn1 N3 150.12(17) . .
Cl1 Zn1 N3 100.38(12) . .
N4 Zn2 Cl4 105.0(2) . .
N4 Zn2 Cl3 105.45(19) . 2_766
Cl4 Zn2 Cl3 115.98(15) . 2_766
N4 Zn2 Cl3 109.32(18) . .
Cl4 Zn2 Cl3 119.82(16) . .
Cl3 Zn2 Cl3 100.49(8) 2_766 .
N4 Zn2 Zn2 117.86(19) . 2_766
Cl4 Zn2 Zn2 137.03(16) . 2_766
Cl3 Zn2 Zn2 50.93(7) 2_766 2_766
Cl3 Zn2 Zn2 49.56(7) . 2_766
C1 N1 C5 118.5(5) . .
C1 N1 Zn1 129.9(4) . .
C5 N1 Zn1 111.6(4) . .
C6 N2 C7 122.4(5) . .
C6 N2 Zn1 118.0(4) . .
C7 N2 Zn1 119.6(4) . .
C9 N3 C12 108.8(5) . .
C9 N3 C8 109.4(5) . .
C12 N3 C8 107.7(5) . .
C9 N3 Zn1 116.6(4) . .
C12 N3 Zn1 114.2(4) . .
C8 N3 Zn1 99.4(3) . .
C10 N4 C11 109.2(5) . .
C10 N4 Zn2 116.2(4) . .
C11 N4 Zn2 113.7(4) . .
C10 N4 H4A 109.8 . .
C11 N4 H4A 109.8 . .
C10 N4 H4B 109.8 . .
C11 N4 H4B 109.8 . .
Zn2 N4 H4B 97.3 . .
H4A N4 H4B 108.3 . .
N1 C1 C2 122.6(6) . .
N1 C1 H1 118.7 . .
C2 C1 H1 118.7 . .
C3 C2 C1 118.7(6) . .
C3 C2 H2 120.6 . .
C1 C2 H2 120.6 . .
C4 C3 C2 119.2(6) . .
C4 C3 H3 120.4 . .
C2 C3 H3 120.4 . .
C3 C4 C5 119.4(6) . .
C3 C4 H4 120.3 . .
C5 C4 H4 120.3 . .
N1 C5 C4 121.6(6) . .
N1 C5 C6 114.7(5) . .
C4 C5 C6 123.7(5) . .
N2 C6 C5 119.9(5) . .
N2 C6 H6 120.0 . .
C5 C6 H6 120.0 . .
N2 C7 C8 107.9(5) . .
N2 C7 H7A 110.1 . .
C8 C7 H7A 110.1 . .
N2 C7 H7B 110.1 . .
C8 C7 H7B 110.1 . .
H7A C7 H7B 108.4 . .
N3 C8 C7 110.8(5) . .
N3 C8 H8A 109.5 . .
C7 C8 H8A 109.5 . .
N3 C8 H8B 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 108.1 . .
N3 C9 C10 112.7(5) . .
N3 C9 H9A 109.0 . .
C10 C9 H9A 109.0 . .
N3 C9 H9B 109.0 . .
C10 C9 H9B 109.0 . .
H9A C9 H9B 107.8 . .
N4 C10 C9 110.4(6) . .
N4 C10 H10A 109.6 . .
C9 C10 H10A 109.6 . .
N4 C10 H10B 109.6 . .
C9 C10 H10B 109.6 . .
H10A C10 H10B 108.1 . .
N4 C11 C12 110.4(6) . .
N4 C11 H11A 109.6 . .
C12 C11 H11A 109.6 . .
N4 C11 H11B 109.6 . .
C12 C11 H11B 109.6 . .
H11A C11 H11B 108.1 . .
N3 C12 C11 112.7(5) . .
N3 C12 H12A 109.1 . .
C11 C12 H12A 109.1 . .
N3 C12 H12B 109.1 . .
C11 C12 H12B 109.1 . .
H12A C12 H12B 107.8 . .
Zn2 Cl3 Zn2 79.51(8) 2_766 .
O2W Cl4 Zn2 109.8(6) 2_776 .
H11W O1W H12W 107.7 . .
Cl4 O2W H21W 128.0 2_776 .
Cl4 O2W H22W 116.4 2_776 .
H21W O2W H22W 101.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N2 2.060(5) .
Zn1 Cl2 2.2360(18) .
Zn1 N1 2.241(5) .
Zn1 Cl1 2.2610(18) .
Zn1 N3 2.481(5) .
Zn2 N4 1.937(6) .
Zn2 Cl4 2.244(5) .
Zn2 Cl3 2.326(3) 2_766
Zn2 Cl3 2.372(3) .
Zn2 Zn2 3.005(3) 2_766
N1 C1 1.326(8) .
N1 C5 1.351(7) .
N2 C6 1.272(8) .
N2 C7 1.444(8) .
N3 C9 1.459(8) .
N3 C12 1.486(8) .
N3 C8 1.488(8) .
N4 C10 1.475(8) .
N4 C11 1.479(9) .
N4 H4A 0.8900 .
N4 H4B 0.8900 .
C1 C2 1.390(9) .
C1 H1 0.9300 .
C2 C3 1.375(9) .
C2 H2 0.9300 .
C3 C4 1.369(9) .
C3 H3 0.9300 .
C4 C5 1.386(9) .
C4 H4 0.9300 .
C5 C6 1.442(9) .
C6 H6 0.9300 .
C7 C8 1.497(10) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C10 1.510(9) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 C12 1.493(10) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
Cl3 Zn2 2.326(3) 2_766
Cl4 O2W 1.33(2) 2_776
O1W H11W 0.8500 .
O1W H12W 0.8500 .
O2W Cl4 1.33(2) 2_776
O2W H21W 0.8905 .
O2W H22W 0.8868 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C5 N1 C1 C2 -0.6(8)
Zn1 N1 C1 C2 178.4(4)
N1 C1 C2 C3 0.6(9)
C1 C2 C3 C4 -0.2(9)
C2 C3 C4 C5 -0.1(9)
C1 N1 C5 C4 0.3(8)
Zn1 N1 C5 C4 -178.8(4)
C1 N1 C5 C6 -179.3(5)
Zn1 N1 C5 C6 1.5(6)
C3 C4 C5 N1 0.0(9)
C3 C4 C5 C6 179.6(5)
C7 N2 C6 C5 177.2(5)
Zn1 N2 C6 C5 -1.3(7)
N1 C5 C6 N2 -0.3(8)
C4 C5 C6 N2 -179.9(5)
C6 N2 C7 C8 -143.8(6)
Zn1 N2 C7 C8 34.6(6)
C9 N3 C8 C7 -74.4(6)
C12 N3 C8 C7 167.5(5)
Zn1 N3 C8 C7 48.2(5)
N2 C7 C8 N3 -57.9(6)
C12 N3 C9 C10 -54.8(7)
C8 N3 C9 C10 -172.2(5)
Zn1 N3 C9 C10 76.0(6)
C11 N4 C10 C9 -57.6(8)
Zn2 N4 C10 C9 172.1(4)
N3 C9 C10 N4 57.8(7)
C10 N4 C11 C12 57.9(7)
Zn2 N4 C11 C12 -170.5(4)
C9 N3 C12 C11 55.1(7)
C8 N3 C12 C11 173.6(5)
Zn1 N3 C12 C11 -77.1(6)
N4 C11 C12 N3 -57.7(7)
