#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100774.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_1100774
loop_
_publ_author_name
'Qiong Ye'
'Yong-Hua Li'
'Yu-Mei Song'
'Xue-Feng Huang'
'Ren-Gen Xiong'
'Ziling Xue'
_publ_section_title
;

A Second-Order Nonlinear Optical Material Prepared through In Situ

Hydrothermal Ligand Synthesis

;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3618
_journal_page_last               3625
_journal_paper_doi               10.1021/ic0500098
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C14 H10 N8 Zn'
_chemical_formula_weight         355.67
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_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                90.00
_cell_formula_units_Z            16
_cell_length_a                   14.2430(18)
_cell_length_b                   14.2430(18)
_cell_length_c                   28.419(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5765.2(14)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            15888
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    1.716
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2880
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.08(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0515P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                2513
_reflns_number_total             3415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0500098si20050104_032035_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 
;
_cod_original_cell_volume        5765.2(15)
_cod_database_code               1100774
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'
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
Zn2 Zn 0.25038(2) 0.2500 0.1250 0.02622(14) Uani 1 2 d S . .
Zn3 Zn 0.5000 0.5000 0.0000 0.02749(16) Uani 1 4 d S . .
N4 N 0.41348(16) 0.43010(17) 0.04266(9) 0.0383(6) Uani 1 1 d . . .
N3 N 0.32705(16) 0.33840(16) 0.08521(9) 0.0344(6) Uani 1 1 d . . .
N2 N 0.17533(15) 0.16799(16) 0.08187(8) 0.0293(5) Uani 1 1 d . . .
C3 C 0.40835(17) 0.34646(18) 0.06315(9) 0.0324(5) Uani 1 1 d . . .
C2 C 0.48292(18) 0.27554(19) 0.06148(9) 0.0374(6) Uani 1 1 d . . .
N7 N 0.17005(15) 0.09590(17) 0.01558(7) 0.0422(6) Uani 1 1 d . . .
N8 N 0.22272(14) 0.14887(17) 0.04122(7) 0.0424(6) Uani 1 1 d . . .
C8 C 0.09260(17) 0.12584(17) 0.07877(8) 0.0264(5) Uani 1 1 d . . .
N9 N 0.08752(14) 0.08041(16) 0.03746(9) 0.0302(5) Uani 1 1 d . . .
Zn1 Zn 0.0000 0.0000 0.0000 0.02384(15) Uani 1 4 d S . .
N1 N 0.28084(15) 0.42141(16) 0.07848(9) 0.0441(6) Uani 1 1 d . . .
C12 C -0.14382(19) 0.1220(2) 0.13573(11) 0.0466(7) Uani 1 1 d . . .
H12A H -0.2065 0.1189 0.1267 0.056 Uiso 1 1 calc R . .
C11 C 0.01854(16) 0.12574(16) 0.11459(8) 0.0280(5) Uani 1 1 d . . .
N6 N 0.33212(16) 0.47536(16) 0.05323(8) 0.0446(6) Uani 1 1 d . . .
C10 C -0.07514(18) 0.12560(18) 0.10198(8) 0.0375(6) Uani 1 1 d . . .
H10A H -0.0917 0.1280 0.0704 0.045 Uiso 1 1 calc R . .
C9 C 0.04235(18) 0.12592(18) 0.16223(8) 0.0369(6) Uani 1 1 d . . .
H9A H 0.1050 0.1267 0.1714 0.044 Uiso 1 1 calc R . .
C13 C -0.1211(2) 0.1228(3) 0.18290(13) 0.0459(7) Uani 1 1 d . . .
H13A H -0.1681 0.1219 0.2056 0.055 Uiso 1 1 calc R . .
C14 C -0.02845(19) 0.1249(2) 0.19582(9) 0.0445(7) Uani 1 1 d . . .
H14A H -0.0127 0.1257 0.2276 0.053 Uiso 1 1 calc R . .
C1 C 0.5773(2) 0.3015(2) 0.06255(11) 0.0520(8) Uani 1 1 d . . .
H1B H 0.5929 0.3645 0.0661 0.062 Uiso 1 1 calc R . .
C7 C 0.6460(2) 0.2377(3) 0.05863(12) 0.0665(10) Uani 1 1 d . . .
H7B H 0.7083 0.2572 0.0596 0.080 Uiso 1 1 calc R . .
C6 C 0.4631(2) 0.1830(2) 0.05641(17) 0.0875(14) Uani 1 1 d . . .
H6B H 0.4010 0.1626 0.0558 0.105 Uiso 1 1 calc R . .
C5 C 0.6265(3) 0.1463(4) 0.0533(2) 0.110(2) Uani 1 1 d . . .
H5A H 0.6741 0.1020 0.0505 0.132 Uiso 1 1 calc R . .
C4 C 0.5340(3) 0.1205(3) 0.0522(3) 0.187(4) Uani 1 1 d . . .
H4A H 0.5193 0.0573 0.0484 0.224 Uiso 1 1 calc R . .
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'
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
N2 Zn2 N2 115.47(11) . 14_454 ?
N2 Zn2 N3 108.08(12) . . ?
N2 Zn2 N3 105.58(9) 14_454 . ?
N2 Zn2 N3 105.58(9) . 14_454 ?
N2 Zn2 N3 108.08(12) 14_454 14_454 ?
N3 Zn2 N3 114.33(12) . 14_454 ?
N4 Zn3 N4 111.68(8) 2_665 3_565 ?
N4 Zn3 N4 111.68(8) 2_665 4_655 ?
N4 Zn3 N4 105.15(15) 3_565 4_655 ?
N4 Zn3 N4 105.15(15) 2_665 . ?
N4 Zn3 N4 111.68(8) 3_565 . ?
N4 Zn3 N4 111.68(8) 4_655 . ?
C3 N4 N6 106.4(2) . . ?
C3 N4 Zn3 138.42(18) . . ?
N6 N4 Zn3 115.10(18) . . ?
C3 N3 N1 106.3(2) . . ?
C3 N3 Zn2 142.71(18) . . ?
N1 N3 Zn2 110.99(17) . . ?
C8 N2 N8 107.0(2) . . ?
C8 N2 Zn2 141.21(18) . . ?
N8 N2 Zn2 111.74(17) . . ?
N3 C3 N4 109.5(2) . . ?
N3 C3 C2 126.2(2) . . ?
N4 C3 C2 124.3(2) . . ?
C6 C2 C1 117.4(3) . . ?
C6 C2 C3 121.5(3) . . ?
C1 C2 C3 121.0(2) . . ?
N8 N7 N9 110.0(2) . . ?
N7 N8 N2 107.9(2) . . ?
N2 C8 N9 108.9(2) . . ?
N2 C8 C11 126.5(2) . . ?
N9 C8 C11 124.6(2) . . ?
C8 N9 N7 106.1(2) . . ?
C8 N9 Zn1 140.83(18) . . ?
N7 N9 Zn1 113.06(18) . . ?
N9 Zn1 N9 106.46(6) . 4 ?
N9 Zn1 N9 106.46(6) . 3 ?
N9 Zn1 N9 115.67(14) 4 3 ?
N9 Zn1 N9 115.67(14) . 2 ?
N9 Zn1 N9 106.46(6) 4 2 ?
N9 Zn1 N9 106.46(6) 3 2 ?
N6 N1 N3 108.8(2) . . ?
C13 C12 C10 120.8(3) . . ?
C13 C12 H12A 119.6 . . ?
C10 C12 H12A 119.6 . . ?
C9 C11 C10 119.1(2) . . ?
C9 C11 C8 119.9(2) . . ?
C10 C11 C8 121.0(2) . . ?
N1 N6 N4 109.0(2) . . ?
C12 C10 C11 120.5(2) . . ?
C12 C10 H10A 119.7 . . ?
C11 C10 H10A 119.7 . . ?
C14 C9 C11 119.4(2) . . ?
C14 C9 H9A 120.3 . . ?
C11 C9 H9A 120.3 . . ?
C14 C13 C12 119.1(3) . . ?
C14 C13 H13A 120.5 . . ?
C12 C13 H13A 120.5 . . ?
C13 C14 C9 121.0(3) . . ?
C13 C14 H14A 119.5 . . ?
C9 C14 H14A 119.5 . . ?
C7 C1 C2 121.5(3) . . ?
C7 C1 H1B 119.2 . . ?
C2 C1 H1B 119.2 . . ?
C5 C7 C1 121.1(3) . . ?
C5 C7 H7B 119.4 . . ?
C1 C7 H7B 119.4 . . ?
C2 C6 C4 119.6(3) . . ?
C2 C6 H6B 120.2 . . ?
C4 C6 H6B 120.2 . . ?
C7 C5 C4 117.6(3) . . ?
C7 C5 H5A 121.2 . . ?
C4 C5 H5A 121.2 . . ?
C6 C4 C5 122.7(4) . . ?
C6 C4 H4A 118.6 . . ?
C5 C4 H4A 118.6 . . ?
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
Zn2 N2 2.002(3) . ?
Zn2 N2 2.002(3) 14_454 ?
Zn2 N3 2.014(3) . ?
Zn2 N3 2.014(3) 14_454 ?
Zn3 N4 1.995(3) 2_665 ?
Zn3 N4 1.995(3) 3_565 ?
Zn3 N4 1.995(3) 4_655 ?
Zn3 N4 1.995(3) . ?
N4 C3 1.328(4) . ?
N4 N6 1.360(3) . ?
N3 C3 1.322(3) . ?
N3 N1 1.367(3) . ?
N2 C8 1.325(3) . ?
N2 N8 1.365(3) . ?
C3 C2 1.466(3) . ?
C2 C6 1.356(4) . ?
C2 C1 1.394(4) . ?
N7 N8 1.290(3) . ?
N7 N9 1.348(3) . ?
C8 N9 1.343(3) . ?
C8 C11 1.466(3) . ?
N9 Zn1 2.000(3) . ?
Zn1 N9 2.000(3) 4 ?
Zn1 N9 2.000(3) 3 ?
Zn1 N9 2.000(3) 2 ?
N1 N6 1.280(3) . ?
C12 C13 1.379(5) . ?
C12 C10 1.371(4) . ?
C12 H12A 0.9300 . ?
C11 C9 1.396(3) . ?
C11 C10 1.382(3) . ?
C10 H10A 0.9300 . ?
C9 C14 1.389(3) . ?
C9 H9A 0.9300 . ?
C13 C14 1.370(4) . ?
C13 H13A 0.9300 . ?
C14 H14A 0.9300 . ?
C1 C7 1.340(4) . ?
C1 H1B 0.9300 . ?
C7 C5 1.339(6) . ?
C7 H7B 0.9300 . ?
C6 C4 1.352(5) . ?
C6 H6B 0.9300 . ?
C5 C4 1.368(6) . ?
C5 H5A 0.9300 . ?
C4 H4A 0.9300 . ?
