#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/33/2003377.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_2003377
loop_
_publ_author_name
'Clegg, W.'
'Hunt, P. A.'
'Straughan, B. P.'
_publ_section_title
;
 Contrasting Structures of Two Adducts of Zinc Crotonate with
 Substituted Pyridines
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              613
_journal_page_last               617
_journal_paper_doi               10.1107/S0108270194011315
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C28 H28 N4 O8 Zn2'
_chemical_formula_weight         679.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0761(6)
_cell_length_b                   12.2729(6)
_cell_length_c                   21.0414(14)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10.0
_cell_volume                     3118.5(3)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988)'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXL93 and local programs'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       Stoe-Siemens
_diffrn_measurement_method
'ω/θ scans with on-line profile fitting (Clegg,'
_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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7471
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        37
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.590
_exptl_absorpt_correction_T_max  0.384
_exptl_absorpt_correction_T_min  0.308
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         .351
_refine_diff_density_min         -.231
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_obs          0.0288
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w = 1/[\s^2^(F~o~^2^) + (0.0398P)^2^ + 1.2129P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0840
_refine_ls_wR_factor_obs         0.0740
_reflns_number_observed          2341
_reflns_number_total             2897
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            mu1144.cif
_cod_data_source_block           zncrotcn
_cod_database_code               2003377
_cod_database_fobs_code          2003377
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
Zn1 1 0.52447(3) 0.2500 0.69454(2) 0.04667(14) Uani d S Zn
Zn2 1 0.54234(3) 0.2500 0.55664(2) 0.04710(14) Uani d S Zn
O11 1 0.6424(2) 0.3640(2) 0.67509(9) 0.0829(7) Uani d . O
O12 1 0.6599(2) 0.3657(2) 0.57082(8) 0.0735(6) Uani d . O
C11 1 0.6866(2) 0.3965(2) 0.62527(11) 0.0560(6) Uani d . C
C12 1 0.7769(2) 0.4772(2) 0.63088(11) 0.0663(7) Uani d . C
H12 1 0.8035(2) 0.5095(2) 0.59393(11) 0.080 Uiso calc R H
C13 1 0.8213(2) 0.5055(3) 0.68502(13) 0.0752(8) Uani d . C
H13 1 0.7912(2) 0.4738(3) 0.72129(13) 0.090 Uiso calc R H
C14 1 0.9146(3) 0.5826(3) 0.6952(2) 0.1075(13) Uani d . C
H14A 1 0.9805(6) 0.5425(4) 0.7054(14) 0.161 Uiso calc R H
H14B 1 0.8969(11) 0.6311(16) 0.7295(10) 0.161 Uiso calc R H
H14C 1 0.9267(17) 0.6241(18) 0.6571(5) 0.161 Uiso calc R H
O21 1 0.4072(2) 0.3660(2) 0.68095(8) 0.0736(6) Uani d . O
O22 1 0.4260(2) 0.3669(2) 0.57673(8) 0.0751(6) Uani d . O
C21 1 0.3833(2) 0.4005(2) 0.62659(11) 0.0558(6) Uani d . C
C22 1 0.2958(3) 0.4835(3) 0.62163(12) 0.0736(8) Uani d . C
H22 1 0.2710(3) 0.5164(3) 0.65883(12) 0.088 Uiso calc R H
C23 1 0.2511(3) 0.5137(3) 0.56796(14) 0.0883(10) Uani d . C
H23 1 0.2793(3) 0.4823(3) 0.53112(14) 0.106 Uiso calc R H
C24 1 0.1591(4) 0.5937(4) 0.5601(2) 0.148(2) Uani d . C
H24A 1 0.0960(12) 0.5577(9) 0.5420(20) 0.222 Uiso calc R H
H24B 1 0.1826(13) 0.6514(19) 0.5324(17) 0.222 Uiso calc R H
H24C 1 0.1397(26) 0.6234(28) 0.6008(4) 0.222 Uiso calc R H
N31 1 0.5367(2) 0.2500 0.79180(13) 0.0465(6) Uani d S N
C31 1 0.6360(3) 0.2500 0.8185(2) 0.0661(11) Uani d S C
H31 1 0.6983(3) 0.2500 0.7925(2) 0.079 Uiso calc SR H
C32 1 0.6505(3) 0.2500 0.8835(2) 0.0616(10) Uani d S C
H32 1 0.7212(3) 0.2500 0.9011(2) 0.074 Uiso calc SR H
C33 1 0.5590(3) 0.2500 0.92135(15) 0.0522(8) Uani d S C
C34 1 0.4558(3) 0.2500 0.8942(2) 0.0717(12) Uani d S C
H34 1 0.3923(3) 0.2500 0.9192(2) 0.086 Uiso calc SR H
C35 1 0.4489(3) 0.2500 0.8294(2) 0.0601(10) Uani d S C
H35 1 0.3790(3) 0.2500 0.8108(2) 0.072 Uiso calc SR H
C36 1 0.5745(4) 0.2500 0.9900(2) 0.0705(11) Uani d S C
N32 1 0.5890(4) 0.2500 1.0429(2) 0.109(2) Uani d S N
N41 1 0.5090(2) 0.2500 0.46086(12) 0.0465(6) Uani d S N
C41 1 0.4909(3) 0.1576(2) 0.43024(11) 0.0666(7) Uani d . C
H41 1 0.5058(3) 0.0923(2) 0.45098(11) 0.080 Uiso calc R H
C42 1 0.4509(3) 0.1538(3) 0.36917(11) 0.0732(9) Uani d . C
H42 1 0.4391(3) 0.0874(3) 0.34895(11) 0.088 Uiso calc R H
C43 1 0.4288(3) 0.2500 0.3387(2) 0.0568(9) Uani d S C
C46 1 0.3808(4) 0.2500 0.2756(2) 0.0783(13) Uani d S C
N42 1 0.3411(4) 0.2500 0.2269(2) 0.116(2) Uani d S N
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C C 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0033 .0016
H H 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0000 .0000
N N 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0061 .0033
O O 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0106 .0060
Zn Zn 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .2839 1.43
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_3
_geom_angle
_geom_angle_publ_flag
O21 Zn1 O21 . 7_565 89.16(13) y
O21 Zn1 O11 . . 88.73(10) y
O21 Zn1 O11 7_565 . 160.30(8) y
O21 Zn1 O11 . 7_565 160.30(8) ?
O21 Zn1 O11 7_565 7_565 88.73(10) ?
O11 Zn1 O11 . 7_565 86.70(14) y
O21 Zn1 N31 . . 101.01(7) y
O21 Zn1 N31 7_565 . 101.01(7) ?
O11 Zn1 N31 . . 98.62(7) y
O11 Zn1 N31 7_565 . 98.62(7) ?
O12 Zn2 O12 . 7_565 88.75(13) y
O12 Zn2 O22 . . 87.68(9) y
O12 Zn2 O22 7_565 . 159.65(7) y
O12 Zn2 O22 . 7_565 159.65(7) ?
O12 Zn2 O22 7_565 7_565 87.68(9) ?
O22 Zn2 O22 . 7_565 88.74(13) y
O12 Zn2 N41 . . 106.33(7) y
O12 Zn2 N41 7_565 . 106.32(7) ?
O22 Zn2 N41 . . 93.90(8) y
O22 Zn2 N41 7_565 . 93.90(8) ?
C11 O11 Zn1 . . 133.7(2) ?
C11 O12 Zn2 . . 121.8(2) ?
O11 C11 O12 . . 124.4(3) ?
O11 C11 C12 . . 117.7(2) ?
O12 C11 C12 . . 117.8(2) ?
C13 C12 C11 . . 123.4(2) ?
C12 C13 C14 . . 127.3(3) ?
C21 O21 Zn1 . . 121.8(2) ?
C21 O22 Zn2 . . 133.8(2) ?
O22 C21 O21 . . 124.4(3) ?
O22 C21 C22 . . 118.0(2) ?
O21 C21 C22 . . 117.6(2) ?
C23 C22 C21 . . 123.7(3) ?
C22 C23 C24 . . 126.2(3) ?
C35 N31 C31 . . 118.2(3) ?
C35 N31 Zn1 . . 122.6(2) ?
C31 N31 Zn1 . . 119.3(2) ?
N31 C31 C32 . . 122.4(3) ?
C33 C32 C31 . . 118.5(3) ?
C32 C33 C34 . . 119.6(3) ?
C32 C33 C36 . . 118.4(3) ?
C34 C33 C36 . . 122.0(3) ?
C35 C34 C33 . . 118.2(3) ?
N31 C35 C34 . . 123.2(3) ?
N32 C36 C33 . . 178.4(5) ?
C41 N41 C41 7_565 . 118.0(3) ?
C41 N41 Zn2 7_565 . 120.69(15) ?
C41 N41 Zn2 . . 120.68(15) ?
N41 C41 C42 . . 122.9(3) ?
C43 C42 C41 . . 118.5(3) ?
C42 C43 C42 7_565 . 119.1(3) ?
C42 C43 C46 7_565 . 120.5(2) ?
C42 C43 C46 . . 120.4(2) ?
N42 C46 C43 . . 178.6(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 O21 . 2.029(2) y
Zn1 O21 7_565 2.029(2) ?
Zn1 O11 . 2.038(2) y
Zn1 O11 7_565 2.038(2) ?
Zn1 N31 . 2.052(3) y
Zn2 O12 . 2.030(2) y
Zn2 O12 7_565 2.030(2) ?
Zn2 O22 . 2.052(2) y
Zn2 O22 7_565 2.052(2) ?
Zn2 N41 . 2.055(3) y
O11 C11 . 1.242(3) ?
O12 C11 . 1.249(3) ?
C11 C12 . 1.477(4) ?
C12 C13 . 1.306(4) ?
C13 C14 . 1.487(4) ?
O21 C21 . 1.253(3) ?
O22 C21 . 1.240(3) ?
C21 C22 . 1.471(4) ?
C22 C23 . 1.305(4) ?
C23 C24 . 1.492(4) ?
N31 C35 . 1.324(4) ?
N31 C31 . 1.325(4) ?
C31 C32 . 1.378(5) ?
C32 C33 . 1.362(5) ?
C33 C34 . 1.371(5) ?
C33 C36 . 1.457(5) ?
C34 C35 . 1.366(5) ?
C36 N32 . 1.126(5) ?
N41 C41 7_565 1.322(3) ?
N41 C41 . 1.322(3) ?
C41 C42 . 1.373(3) ?
C42 C43 . 1.370(3) ?
C43 C42 7_565 1.370(3) ?
C43 C46 . 1.449(5) ?
C46 N42 . 1.132(5) ?
