#------------------------------------------------------------------------------
#$Date: 2018-08-14 18:55:18 +0300 (Tue, 14 Aug 2018) $
#$Revision: 209691 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/37/7113790.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_7113790
loop_
_publ_author_name
'Puerta, David T.'
'Cohen, Seth M.'
_publ_section_title
;
 Synthesis and structure of the hexameric, dodecanuclear metallamacrocycle
 [(5-methyl-3-phenylpyrazole)2Zn2(OCH2CH2S)]6
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   11
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1278
_journal_page_last               1279
_journal_paper_doi               10.1039/b300453h
_journal_year                    2003
_chemical_formula_moiety         '[Zn6(5,3-mppz)6(b-me)]2'
_chemical_formula_sum            'C132 H132 N24 O6 S6 Zn12'
_chemical_formula_weight         3127.42
_chemical_name_systematic
;
[(5,3-methylphenylpyrazole)2Zn2(OCH2CH2S)]6
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   29.6563(18)
_cell_length_b                   29.6563(18)
_cell_length_c                   19.187(3)
_cell_measurement_temperature    100(2)
_cell_volume                     14614(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.706
_diffrn_measured_fraction_theta_max 0.706
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.1274
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24253
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    1.556
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             4788
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         5294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          25.056
_refine_ls_shift/su_mean         0.116
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0907P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1949
_refine_ls_wR_factor_ref         0.2001
_reflns_number_gt                3177
_reflns_number_total             5294
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103663
_cod_data_source_file            b300453h.txt
_cod_data_source_block           finalring
_cod_original_cell_volume        14614(2)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7113790
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Zn2 Zn 0.11776(2) 0.46100(2) 0.19670(3) 0.0329(2) Uani 1 1 d .
Zn1 Zn 0.21057(3) 0.43307(3) 0.17526(3) 0.0365(2) Uani 1 1 d .
S1 S 0.15527(6) 0.44484(6) 0.10058(8) 0.0438(4) Uani 1 1 d .
N2 N 0.14673(18) 0.44557(18) 0.2798(2) 0.0341(9) Uani 1 1 d .
N1 N 0.18154(18) 0.42849(19) 0.2705(2) 0.0379(10) Uani 1 1 d .
C2 C 0.1909(2) 0.4139(2) 0.3328(3) 0.0431(13) Uani 1 1 d .
C1 C 0.2282(3) 0.3938(4) 0.3395(4) 0.0610(19) Uani 1 1 d .
H1A H 0.2341 0.3832 0.2936 0.092 Uiso 1 1 calc R
H1B H 0.2136 0.3638 0.3711 0.092 Uiso 1 1 calc R
H1C H 0.2614 0.4213 0.3583 0.092 Uiso 1 1 calc R
C4 C 0.1346(2) 0.4412(2) 0.3474(3) 0.0401(12) Uani 1 1 d .
C3 C 0.1619(3) 0.4203(3) 0.3819(3) 0.0525(16) Uani 1 1 d .
H3 H 0.1603 0.4124 0.4302 0.063 Uiso 1 1 calc R
N3 N 0.21702(18) 0.37202(19) 0.1438(2) 0.0374(10) Uani 1 1 d .
C5 C 0.0980(3) 0.4576(2) 0.3741(3) 0.0421(13) Uani 1 1 d .
C12 C 0.1819(2) 0.3235(2) 0.1219(3) 0.0423(13) Uani 1 1 d .
C11 C 0.1260(3) 0.3053(3) 0.1255(4) 0.0561(16) Uani 1 1 d .
H11A H 0.1204 0.3297 0.1535 0.084 Uiso 1 1 calc R
H11B H 0.1078 0.2707 0.1471 0.084 Uiso 1 1 calc R
H11C H 0.1124 0.3034 0.0784 0.084 Uiso 1 1 calc R
C13 C 0.2068(2) 0.2990(2) 0.0965(3) 0.0421(13) Uani 1 1 d .
H13 H 0.1915 0.2651 0.0771 0.051 Uiso 1 1 calc R
C10 C 0.0983(3) 0.5013(2) 0.3470(3) 0.0444(13) Uani 1 1 d .
H10 H 0.1230 0.5216 0.3123 0.053 Uiso 1 1 calc R
C6 C 0.0631(3) 0.4298(3) 0.4267(3) 0.0569(17) Uani 1 1 d .
H6 H 0.0631 0.4004 0.4464 0.068 Uiso 1 1 calc R
C9 C 0.0634(3) 0.5150(3) 0.3700(3) 0.0553(17) Uani 1 1 d .
H9 H 0.0631 0.5441 0.3496 0.066 Uiso 1 1 calc R
C8 C 0.0286(3) 0.4875(3) 0.4223(4) 0.0609(19) Uani 1 1 d .
H8 H 0.0050 0.4979 0.4388 0.073 Uiso 1 1 calc R
C7 C 0.0284(3) 0.4441(3) 0.4507(4) 0.065(2) Uani 1 1 d .
H7 H 0.0044 0.4246 0.4866 0.078 Uiso 1 1 calc R
N4 N 0.26533(18) 0.37914(18) 0.1341(2) 0.0350(9) Uani 1 1 d .
C14 C 0.2603(2) 0.3349(2) 0.1050(3) 0.0372(11) Uani 1 1 d .
C15 C 0.3056(2) 0.3297(2) 0.0891(3) 0.0403(12) Uani 1 1 d .
C16 C 0.3060(3) 0.3024(3) 0.0309(3) 0.0494(15) Uani 1 1 d .
H16 H 0.2770 0.2880 0.0002 0.059 Uiso 1 1 calc R
C20 C 0.3492(2) 0.3504(2) 0.1330(3) 0.0417(12) Uani 1 1 d .
H20 H 0.3508 0.3702 0.1728 0.050 Uiso 1 1 calc R
C22 C 0.1930(3) 0.5504(3) 0.1383(6) 0.075(3) Uani 1 1 d .
H22A H 0.2206 0.5532 0.1700 0.091 Uiso 1 1 calc R
H22B H 0.2044 0.5857 0.1199 0.091 Uiso 1 1 calc R
C19 C 0.3896(2) 0.3418(2) 0.1182(4) 0.0488(14) Uani 1 1 d .
H19 H 0.4186 0.3552 0.1489 0.059 Uiso 1 1 calc R
C18 C 0.3893(3) 0.3151(2) 0.0618(4) 0.0570(19) Uani 1 1 d .
H18 H 0.4176 0.3095 0.0530 0.068 Uiso 1 1 calc R
C21 C 0.1882(3) 0.5134(3) 0.0743(4) 0.0547(16) Uani 1 1 d .
H21A H 0.2234 0.5237 0.0566 0.066 Uiso 1 1 calc R
H21B H 0.1684 0.5180 0.0360 0.066 Uiso 1 1 calc R
C17 C 0.3479(3) 0.2959(3) 0.0170(4) 0.0576(18) Uani 1 1 d .
H17 H 0.3481 0.2779 -0.0240 0.069 Uiso 1 1 calc R
O1 O 0.1534(2) 0.53610(18) 0.1719(2) 0.0485(11) 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'
S S 0.1246 0.1234 '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
N4 Zn2 N2 119.06(18) 14_455 .
N4 Zn2 O1 98.9(2) 14_455 .
N2 Zn2 O1 113.83(19) . .
N4 Zn2 S1 124.02(14) 14_455 .
N2 Zn2 S1 106.58(14) . .
O1 Zn2 S1 89.99(13) . .
O1 Zn1 N1 116.33(19) 15 .
O1 Zn1 N3 97.08(19) 15 .
N1 Zn1 N3 116.53(19) . .
O1 Zn1 S1 111.82(14) 15 .
N1 Zn1 S1 105.14(14) . .
N3 Zn1 S1 109.99(14) . .
C21 S1 Zn2 92.0(2) . .
C21 S1 Zn1 108.1(2) . .
Zn2 S1 Zn1 89.32(6) . .
C4 N2 N1 107.9(5) . .
C4 N2 Zn2 132.9(4) . .
N1 N2 Zn2 118.4(3) . .
C2 N1 N2 108.4(4) . .
C2 N1 Zn1 133.2(4) . .
N2 N1 Zn1 118.3(3) . .
N1 C2 C3 109.1(5) . .
N1 C2 C1 121.0(6) . .
C3 C2 C1 130.0(6) . .
N2 C4 C3 108.3(5) . .
N2 C4 C5 120.6(5) . .
C3 C4 C5 131.1(6) . .
C2 C3 C4 106.3(6) . .
N4 N3 C12 108.3(5) . .
N4 N3 Zn1 118.2(4) . .
C12 N3 Zn1 133.1(4) . .
C6 C5 C10 118.9(6) . .
C6 C5 C4 120.4(6) . .
C10 C5 C4 120.8(5) . .
N3 C12 C13 110.2(5) . .
N3 C12 C11 120.1(6) . .
C13 C12 C11 129.6(6) . .
C12 C13 C14 105.2(5) . .
C9 C10 C5 120.4(6) . .
C7 C6 C5 120.7(6) . .
C10 C9 C8 121.0(6) . .
C9 C8 C7 119.2(7) . .
C6 C7 C8 119.8(6) . .
N3 N4 C14 108.0(5) . .
N3 N4 Zn2 116.9(4) . 15
C14 N4 Zn2 132.1(4) . 15
N4 C14 C13 108.3(5) . .
N4 C14 C15 121.6(5) . .
C13 C14 C15 130.1(5) . .
C16 C15 C20 117.7(6) . .
C16 C15 C14 120.6(6) . .
C20 C15 C14 121.7(5) . .
C17 C16 C15 120.8(7) . .
C19 C20 C15 119.6(6) . .
O1 C22 C21 115.4(6) . .
C18 C19 C20 121.9(7) . .
C19 C18 C17 119.6(6) . .
C22 C21 S1 111.3(5) . .
C18 C17 C16 120.3(6) . .
C22 O1 Zn1 127.5(4) . 14_455
C22 O1 Zn2 113.4(4) . .
Zn1 O1 Zn2 108.0(3) 14_455 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn2 N4 1.962(5) 14_455
Zn2 N2 1.971(5) .
Zn2 O1 1.987(5) .
Zn2 S1 2.3241(16) .
Zn1 O1 1.970(5) 15
Zn1 N1 1.995(5) .
Zn1 N3 2.006(5) .
Zn1 S1 2.3319(17) .
S1 C21 1.833(8) .
N2 C4 1.335(7) .
N2 N1 1.370(6) .
N1 C2 1.347(7) .
C2 C3 1.352(10) .
C2 C1 1.503(9) .
C4 C3 1.406(9) .
C4 C5 1.486(9) .
N3 N4 1.353(6) .
N3 C12 1.355(8) .
C5 C6 1.385(9) .
C5 C10 1.391(9) .
C12 C13 1.357(9) .
C12 C11 1.468(9) .
C13 C14 1.410(8) .
C10 C9 1.360(10) .
C6 C7 1.375(11) .
C9 C8 1.378(10) .
C8 C7 1.394(11) .
N4 C14 1.364(7) .
N4 Zn2 1.962(5) 15
C14 C15 1.458(8) .
C15 C16 1.382(8) .
C15 C20 1.402(9) .
C16 C17 1.377(10) .
C20 C19 1.372(9) .
C22 O1 1.216(11) .
C22 C21 1.603(13) .
C19 C18 1.339(9) .
C18 C17 1.368(11) .
O1 Zn1 1.971(5) 14_455
