#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:08:46 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179828 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/24/7012436.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_7012436
loop_
_publ_author_name
'Atkins, Andrew J.'
'Black, Daniel'
'Finn, Rachel L.'
'Marin-Becerra, Armando'
'Blake, Alexander J.'
'Ruiz-Ramirez, Lena'
'Li, Wan-Sheung'
'Schröder, Martin'
_publ_section_title
;
 Synthesis and structure of mononuclear and binuclear zinc(ii)
 compartmental macrocyclic complexes
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1730
_journal_paper_doi               10.1039/b210936k
_journal_year                    2003
_chemical_formula_moiety         'C30 H36 N4 O6 Zn2, C H Cl3'
_chemical_formula_sum            'C31 H37 Cl3 N4 O6 Zn2'
_chemical_formula_weight         798.74
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.75(3)
_cell_angle_beta                 96.16(3)
_cell_angle_gamma                108.63(3)
_cell_formula_units_Z            2
_cell_length_a                   11.565(7)
_cell_length_b                   12.732(3)
_cell_length_c                   13.289(2)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.15
_cell_measurement_theta_min      16
_cell_volume                     1649.2(13)
_computing_cell_refinement       'Stadi-4 (Stoe & Cie, 1995a)'
_computing_data_collection       'Stadi-4 (Stoe & Cie, 1995a)'
_computing_data_reduction        'X-red (Stoe & Cie, 1995b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.797
_diffrn_measured_fraction_theta_max 0.797
_diffrn_measurement_device_type  'Stoe Stadi-4 four circle'
_diffrn_measurement_method       Omega-theta
_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  0.099
_diffrn_reflns_av_sigmaI/netI    0.057
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5093
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.90
_diffrn_standards_decay_%        13
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.747
_exptl_absorpt_correction_T_max  0.559
_exptl_absorpt_correction_T_min  0.453
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.86
_refine_diff_density_rms         0.15
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         4650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.054P)²+21.64P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.163
_refine_ls_wR_factor_ref         0.187
_reflns_number_gt                3524
_reflns_number_total             4650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210936k.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1649.2(11)
_cod_database_code               7012436
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.30024(10) 0.11312(10) -0.32574(9) 0.0192(3) Uani 1 1 d . . .
Zn2 Zn 0.33385(9) 0.23364(10) -0.06492(9) 0.0199(3) Uani 1 1 d . . .
O1 O 0.2818(5) 0.2664(6) -0.2024(5) 0.0190(14) Uani 1 1 d . . .
O2 O 0.4280(5) 0.1634(6) -0.1712(5) 0.0223(14) Uani 1 1 d . . .
O3 O 0.2884(6) -0.0574(6) -0.4315(5) 0.0280(16) Uani 1 1 d . . .
O4 O 0.2375(7) -0.2587(6) -0.5006(6) 0.0329(17) Uani 1 1 d . . .
O5 O 0.1432(6) 0.0059(6) -0.2725(5) 0.0257(15) Uani 1 1 d . . .
O6 O 0.1769(6) 0.1000(6) -0.0841(5) 0.0258(15) Uani 1 1 d . . .
N1 N 0.1751(7) 0.1260(7) -0.4418(6) 0.0192(17) Uani 1 1 d . . .
N2 N 0.4697(7) 0.1959(7) -0.3621(6) 0.0221(18) Uani 1 1 d . . .
N3 N 0.3577(7) 0.4110(7) 0.0310(6) 0.0222(18) Uani 1 1 d . . .
N4 N 0.4450(7) 0.2145(7) 0.0591(6) 0.0197(17) Uani 1 1 d . . .
C1 C 0.1977(8) 0.3149(9) -0.2040(8) 0.022(2) Uani 1 1 d . . .
C2 C 0.1045(9) 0.2731(9) -0.3054(8) 0.022(2) Uani 1 1 d . . .
C3 C 0.0156(8) 0.3286(9) -0.3024(8) 0.022(2) Uani 1 1 d . . .
H3 H -0.0482 0.2983 -0.3697 0.026 Uiso 1 1 calc R . .
C4 C 0.0178(9) 0.4242(9) -0.2065(8) 0.026(2) Uani 1 1 d . . .
C5 C 0.1135(9) 0.4687(9) -0.1103(8) 0.024(2) Uani 1 1 d . . .
H5 H 0.1206 0.5388 -0.0445 0.029 Uiso 1 1 calc R . .
C6 C 0.1997(8) 0.4141(8) -0.1068(7) 0.018(2) Uani 1 1 d . . .
C7 C -0.0759(10) 0.4843(10) -0.2080(9) 0.036(3) Uani 1 1 d . . .
H7A H -0.0336 0.5646 -0.2077 0.054 Uiso 1 1 calc R . .
H7B H -0.1083 0.4966 -0.1410 0.054 Uiso 1 1 calc R . .
H7C H -0.1462 0.4306 -0.2764 0.054 Uiso 1 1 calc R . .
C8 C 0.1005(9) 0.1831(8) -0.4162(8) 0.024(2) Uani 1 1 d . . .
H8 H 0.0344 0.1642 -0.4774 0.029 Uiso 1 1 calc R . .
C9 C 0.1538(9) 0.0471(9) -0.5630(7) 0.024(2) Uani 1 1 d . . .
H9A H 0.0684 0.0299 -0.6046 0.029 Uiso 1 1 calc R . .
H9B H 0.1573 -0.0330 -0.5733 0.029 Uiso 1 1 calc R . .
C10 C 0.2521(9) 0.1085(10) -0.6119(8) 0.028(2) Uani 1 1 d . . .
H10A H 0.2515 0.1910 -0.5958 0.034 Uiso 1 1 calc R . .
H10B H 0.2256 0.0586 -0.6951 0.034 Uiso 1 1 calc R . .
C11 C 0.3883(9) 0.1258(10) -0.5690(8) 0.033(3) Uani 1 1 d . . .
H11A H 0.3864 0.0488 -0.5660 0.040 Uiso 1 1 calc R . .
H11B H 0.4348 0.1363 -0.6252 0.040 Uiso 1 1 calc R . .
C12 C 0.4627(9) 0.2341(9) -0.4537(8) 0.028(2) Uani 1 1 d . . .
H12A H 0.5496 0.2759 -0.4569 0.034 Uiso 1 1 calc R . .
H12B H 0.4224 0.2947 -0.4359 0.034 Uiso 1 1 calc R . .
C13 C 0.5801(8) 0.2019(8) -0.3228(7) 0.022(2) Uani 1 1 d . . .
H13 H 0.6422 0.2203 -0.3617 0.026 Uiso 1 1 calc R . .
C14 C 0.6188(8) 0.1836(8) -0.2255(8) 0.020(2) Uani 1 1 d . . .
C15 C 0.7413(8) 0.1853(9) -0.2016(8) 0.024(2) Uani 1 1 d . . .
H15 H 0.7900 0.1896 -0.2541 0.029 Uiso 1 1 calc R . .
C16 C 0.7942(8) 0.1809(9) -0.1060(8) 0.026(2) Uani 1 1 d . . .
C17 C 0.7249(9) 0.1808(9) -0.0282(8) 0.026(2) Uani 1 1 d . . .
H17 H 0.7615 0.1813 0.0396 0.031 Uiso 1 1 calc R . .
C18 C 0.6027(8) 0.1801(9) -0.0443(7) 0.021(2) Uani 1 1 d . . .
C19 C 0.5446(8) 0.1739(8) -0.1488(8) 0.019(2) Uani 1 1 d . . .
C20 C 0.9251(9) 0.1810(11) -0.0840(9) 0.037(3) Uani 1 1 d . . .
H20A H 0.9493 0.1545 -0.1554 0.055 Uiso 1 1 calc R . .
H20B H 0.9255 0.1239 -0.0515 0.055 Uiso 1 1 calc R . .
H20C H 0.9857 0.2648 -0.0310 0.055 Uiso 1 1 calc R . .
C21 C 0.5435(8) 0.1916(9) 0.0475(8) 0.023(2) Uani 1 1 d . . .
H21 H 0.5831 0.1806 0.1070 0.027 Uiso 1 1 calc R . .
C22 C 0.4007(10) 0.2214(10) 0.1603(9) 0.035(3) Uani 1 1 d . . .
H22A H 0.4750 0.2564 0.2254 0.042 Uiso 1 1 calc R . .
H22B H 0.3488 0.1365 0.1478 0.042 Uiso 1 1 calc R . .
C23 C 0.3239(9) 0.2991(10) 0.1892(8) 0.031(2) Uani 1 1 d . . .
H23A H 0.2868 0.2878 0.2499 0.038 Uiso 1 1 calc R . .
H23B H 0.2527 0.2650 0.1218 0.038 Uiso 1 1 calc R . .
C24 C 0.3899(9) 0.4392(9) 0.2276(8) 0.025(2) Uani 1 1 d . . .
H24A H 0.3272 0.4765 0.2463 0.030 Uiso 1 1 calc R . .
H24B H 0.4571 0.4749 0.2982 0.030 Uiso 1 1 calc R . .
C25 C 0.4490(8) 0.4789(9) 0.1443(8) 0.027(2) Uani 1 1 d . . .
H25A H 0.4734 0.5692 0.1714 0.032 Uiso 1 1 calc R . .
H25B H 0.5263 0.4616 0.1392 0.032 Uiso 1 1 calc R . .
C26 C 0.2942(8) 0.4673(8) 0.0024(8) 0.021(2) Uani 1 1 d . . .
H26 H 0.3097 0.5492 0.0557 0.025 Uiso 1 1 calc R . .
C27 C 0.2793(8) -0.1526(10) -0.4197(8) 0.024(2) Uani 1 1 d . . .
C28 C 0.3161(11) -0.1426(10) -0.3025(8) 0.039(3) Uani 1 1 d . . .
H28A H 0.2399 -0.1799 -0.2821 0.058 Uiso 1 1 calc R . .
H28B H 0.3603 -0.0551 -0.2479 0.058 Uiso 1 1 calc R . .
H28C H 0.3721 -0.1862 -0.3018 0.058 Uiso 1 1 calc R . .
C29 C 0.1176(9) 0.0113(9) -0.1818(9) 0.026(2) Uani 1 1 d . . .
C30 C 0.0146(9) -0.1001(9) -0.1862(9) 0.031(2) Uani 1 1 d . . .
H30A H -0.0539 -0.1371 -0.2551 0.047 Uiso 1 1 calc R . .
H30B H -0.0184 -0.0743 -0.1198 0.047 Uiso 1 1 calc R . .
H30C H 0.0492 -0.1611 -0.1865 0.047 Uiso 1 1 calc R . .
C1S C 0.2197(11) 0.5195(10) -0.4589(9) 0.040(3) Uani 1 1 d . . .
H1S H 0.2157 0.5920 -0.4696 0.047 Uiso 1 1 calc R . .
Cl1 Cl 0.0821(3) 0.3912(3) -0.5423(3) 0.0672(11) Uani 1 1 d . . .
Cl2 Cl 0.3532(3) 0.4935(3) -0.4987(3) 0.0592(9) Uani 1 1 d . . .
Cl3 Cl 0.2399(3) 0.5556(3) -0.3147(2) 0.0527(9) 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'
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
_geom_angle_publ_flag
O3 Zn1 N1 95.9(3) . . ?
O3 Zn1 O1 166.7(3) . . ?
N1 Zn1 O1 86.2(3) . . ?
O3 Zn1 N2 90.2(3) . . ?
N1 Zn1 N2 98.2(3) . . ?
O1 Zn1 N2 102.5(3) . . ?
O3 Zn1 O2 104.8(3) . . ?
N1 Zn1 O2 159.4(3) . . ?
O1 Zn1 O2 73.7(2) . . ?
N2 Zn1 O2 82.3(3) . . ?
O3 Zn1 O5 83.9(3) . . ?
N1 Zn1 O5 93.3(3) . . ?
O1 Zn1 O5 82.9(2) . . ?
N2 Zn1 O5 167.6(3) . . ?
O2 Zn1 O5 88.7(2) . . ?
O3 Zn1 Zn2 129.97(19) . . ?
N1 Zn1 Zn2 124.2(2) . . ?
O1 Zn1 Zn2 41.87(16) . . ?
N2 Zn1 Zn2 109.7(2) . . ?
O2 Zn1 Zn2 39.08(16) . . ?
O5 Zn1 Zn2 66.89(17) . . ?
O6 Zn2 O2 109.2(3) . . ?
O6 Zn2 N3 118.4(3) . . ?
O2 Zn2 N3 131.3(3) . . ?
O6 Zn2 O1 100.8(3) . . ?
O2 Zn2 O1 76.8(2) . . ?
N3 Zn2 O1 85.0(3) . . ?
O6 Zn2 N4 95.0(3) . . ?
O2 Zn2 N4 87.5(3) . . ?
N3 Zn2 N4 97.3(3) . . ?
O1 Zn2 N4 160.6(3) . . ?
O6 Zn2 Zn1 90.17(19) . . ?
O2 Zn2 Zn1 42.49(17) . . ?
N3 Zn2 Zn1 125.2(2) . . ?
O1 Zn2 Zn1 41.97(16) . . ?
N4 Zn2 Zn1 127.7(2) . . ?
C1 O1 Zn2 120.1(5) . . ?
C1 O1 Zn1 131.5(6) . . ?
Zn2 O1 Zn1 96.2(2) . . ?
C19 O2 Zn2 128.6(6) . . ?
C19 O2 Zn1 131.2(6) . . ?
Zn2 O2 Zn1 98.4(2) . . ?
C27 O3 Zn1 133.7(6) . . ?
C29 O5 Zn1 137.3(6) . . ?
C29 O6 Zn2 119.7(6) . . ?
C8 N1 C9 116.3(7) . . ?
C8 N1 Zn1 125.1(6) . . ?
C9 N1 Zn1 117.8(6) . . ?
C13 N2 C12 114.3(8) . . ?
C13 N2 Zn1 126.2(6) . . ?
C12 N2 Zn1 118.8(6) . . ?
C26 N3 C25 117.7(8) . . ?
C26 N3 Zn2 124.5(6) . . ?
C25 N3 Zn2 117.7(6) . . ?
C21 N4 C22 119.1(8) . . ?
C21 N4 Zn2 123.3(6) . . ?
C22 N4 Zn2 117.5(6) . . ?
O1 C1 C6 121.3(8) . . ?
O1 C1 C2 121.3(8) . . ?
C6 C1 C2 117.4(8) . . ?
C3 C2 C1 119.0(8) . . ?
C3 C2 C8 116.7(8) . . ?
C1 C2 C8 124.0(8) . . ?
C4 C3 C2 122.8(9) . . ?
C3 C4 C5 117.5(8) . . ?
C3 C4 C7 121.1(9) . . ?
C5 C4 C7 121.2(9) . . ?
C4 C5 C6 122.1(9) . . ?
C5 C6 C1 121.0(8) . . ?
C5 C6 C26 116.9(8) . . ?
C1 C6 C26 122.2(8) . . ?
N1 C8 C2 128.5(8) . . ?
N1 C9 C10 111.5(8) . . ?
C9 C10 C11 116.7(8) . . ?
C12 C11 C10 116.3(8) . . ?
N2 C12 C11 112.9(8) . . ?
N2 C13 C14 126.6(8) . . ?
C15 C14 C19 118.4(8) . . ?
C15 C14 C13 117.7(8) . . ?
C19 C14 C13 123.7(8) . . ?
C16 C15 C14 123.5(8) . . ?
C17 C16 C15 117.5(8) . . ?
C17 C16 C20 120.5(9) . . ?
C15 C16 C20 122.0(9) . . ?
C16 C17 C18 123.0(9) . . ?
C17 C18 C19 118.8(8) . . ?
C17 C18 C21 118.2(8) . . ?
C19 C18 C21 123.0(8) . . ?
O2 C19 C14 120.6(8) . . ?
O2 C19 C18 121.0(8) . . ?
C14 C19 C18 118.4(7) . . ?
N4 C21 C18 128.4(8) . . ?
N4 C22 C23 113.0(8) . . ?
C22 C23 C24 118.6(8) . . ?
C25 C24 C23 116.9(8) . . ?
N3 C25 C24 110.1(7) . . ?
N3 C26 C6 125.1(8) . . ?
O4 C27 O3 123.2(9) . . ?
O4 C27 C28 116.8(9) . . ?
O3 C27 C28 119.9(9) . . ?
O5 C29 O6 125.4(9) . . ?
O5 C29 C30 118.1(9) . . ?
O6 C29 C30 116.2(8) . . ?
Cl1 C1S Cl3 111.7(6) . . ?
Cl1 C1S Cl2 110.5(6) . . ?
Cl3 C1S Cl2 108.2(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N1 2.090(7) . ?
Zn1 N2 2.112(8) . ?
Zn1 O1 2.099(6) . ?
Zn1 O2 2.131(6) . ?
Zn1 O3 2.028(6) . ?
Zn2 N3 2.025(8) . ?
Zn2 N4 2.117(7) . ?
Zn2 O1 2.094(6) . ?
Zn2 O2 1.988(6) . ?
Zn1 O5 2.259(6) . ?
Zn2 O6 1.961(6) . ?
Zn1 Zn2 3.120(2) . ?
O1 C1 1.311(11) . ?
O2 C19 1.302(10) . ?
O3 C27 1.256(12) . ?
O4 C27 1.249(12) . ?
O5 C29 1.254(11) . ?
O6 C29 1.269(12) . ?
N1 C8 1.288(12) . ?
N1 C9 1.473(11) . ?
N2 C13 1.293(11) . ?
N2 C12 1.480(12) . ?
N3 C26 1.300(12) . ?
N3 C25 1.482(11) . ?
N4 C21 1.274(11) . ?
N4 C22 1.471(12) . ?
C1 C6 1.406(13) . ?
C1 C2 1.424(13) . ?
C2 C3 1.417(12) . ?
C2 C8 1.460(13) . ?
C3 C4 1.371(13) . ?
C4 C5 1.385(13) . ?
C4 C7 1.516(13) . ?
C5 C6 1.391(12) . ?
C6 C26 1.478(12) . ?
C9 C10 1.520(13) . ?
C10 C11 1.531(13) . ?
C11 C12 1.521(14) . ?
C13 C14 1.450(13) . ?
C14 C15 1.410(12) . ?
C14 C19 1.417(13) . ?
C15 C16 1.379(14) . ?
C16 C17 1.374(13) . ?
C16 C20 1.511(13) . ?
C17 C18 1.403(12) . ?
C18 C19 1.438(13) . ?
C18 C21 1.443(13) . ?
C22 C23 1.503(14) . ?
C23 C24 1.539(14) . ?
C24 C25 1.524(13) . ?
C27 C28 1.513(13) . ?
C29 C30 1.508(14) . ?
C1S Cl1 1.729(12) . ?
C1S Cl3 1.759(11) . ?
C1S Cl2 1.772(12) . ?
