#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:22:51 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180426 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/95/7209509.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_7209509
loop_
_publ_author_name
'Schröder, Christian A.'
'Baburin, Igor A.'
'van Wüllen, Leo'
'Wiebcke, Michael'
'Leoni, Stefano'
_publ_section_title
;
 Subtle polymorphism of zinc imidazolate frameworks: temperature-dependent
 ground states in the energy landscape revealed by experiment and theory
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              4036
_journal_paper_doi               10.1039/c2ce26045j
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         '2(C6 H6 N4 Zn), C5 H5 N'
_chemical_formula_sum            'C17 H17 N9 Zn2'
_chemical_formula_weight         478.14
_chemical_melting_point          'ca. 410 C (decomp.)'
_chemical_name_common            diimidazolatozinc(ii)
_chemical_name_systematic
;
diimidazolatozinc(II)
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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            8
_cell_length_a                   18.50490(10)
_cell_length_b                   23.8735(2)
_cell_length_c                   9.31560(10)
_cell_measurement_reflns_used    8186
_cell_measurement_temperature    173
_cell_measurement_theta_max      65.326
_cell_measurement_theta_min      4.772
_cell_volume                     4115.42(6)
_computing_cell_refinement       'SAINT (BRUKER, 2006)'
_computing_data_collection       'APEX2 (BRUKER, 2006)'
_computing_data_reduction        'SAINT (BRUKER, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER Kappa Apex II CCD'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8941
_diffrn_reflns_theta_full        65.40
_diffrn_reflns_theta_max         65.40
_diffrn_reflns_theta_min         5.63
_exptl_absorpt_coefficient_mu    3.047
_exptl_absorpt_correction_T_max  0.7386
_exptl_absorpt_correction_T_min  0.5796
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (BRUKER, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1710
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0479P)²+5.3652P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0732
_reflns_number_gt                1696
_reflns_number_total             1710
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26045j.txt
_cod_data_source_block           nebpy
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               7209509
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+3/4, -y+5/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+5/4, -y+3/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+5/4, -y+5/4, z+1/4'
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
Zn Zn 0.045857(17) 0.314894(14) 0.70762(5) 0.03334(14) Uani 1 1 d .
N1 N -0.00210(14) 0.30293(11) 0.5186(3) 0.0388(5) Uani 1 1 d .
C2 C -0.01159(15) 0.25280(13) 0.4593(4) 0.0381(6) Uani 1 1 d .
H2 H -0.0021 0.2194 0.5071 0.046 Uiso 1 1 calc R
N3 N 0.03582(14) 0.24504(11) 0.8262(3) 0.0393(6) Uani 1 1 d .
C4 C -0.04229(19) 0.31068(14) 0.2970(4) 0.0475(9) Uani 1 1 d .
H4 H -0.0584 0.3259 0.2108 0.057 Uiso 1 1 calc R
C5 C -0.02146(18) 0.34013(13) 0.4139(4) 0.0448(7) Uani 1 1 d .
H5 H -0.0205 0.3790 0.4218 0.054 Uiso 1 1 calc R
N6 N -0.00723(13) 0.37203(10) 0.8223(3) 0.0355(5) Uani 1 1 d .
C7 C -0.07818(15) 0.38148(12) 0.8168(3) 0.0341(6) Uani 1 1 d .
H7 H -0.1081 0.3669 0.7459 0.041 Uiso 1 1 calc R
N8 N 0.14815(12) 0.33604(10) 0.6732(3) 0.0338(5) Uani 1 1 d .
C9 C -0.04194(16) 0.42651(13) 1.0033(4) 0.0396(7) Uani 1 1 d .
H9 H -0.0407 0.4489 1.0849 0.048 Uiso 1 1 calc R
C10 C 0.01550(15) 0.40023(13) 0.9417(4) 0.0418(7) Uani 1 1 d .
H10 H 0.0628 0.4013 0.9756 0.050 Uiso 1 1 calc R
N11 N 0.0000 0.5000 1.3371(6) 0.0795(18) Uani 1 2 d S
C12 C -0.0593(3) 0.5011(2) 1.4095(8) 0.0860(19) Uani 1 1 d .
H12 H -0.1027 0.5022 1.3592 0.103 Uiso 1 1 calc R
C13 C -0.0620(4) 0.5009(2) 1.5533(9) 0.104(3) Uani 1 1 d .
H13 H -0.1061 0.5013 1.6010 0.125 Uiso 1 1 calc R
C14 C 0.0000 0.5000 1.6267(7) 0.108(4) Uani 1 2 d S
H14 H 0.0000 0.5000 1.7266 0.130 Uiso 1 2 calc SR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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
N8 Zn N6 112.51(10) . .
N8 Zn N1 108.56(11) . .
N6 Zn N1 110.65(11) . .
N8 Zn N3 112.84(10) . .
N6 Zn N3 103.18(11) . .
N1 Zn N3 109.00(11) . .
C2 N1 C5 104.7(3) . .
C2 N1 Zn 123.7(2) . .
C5 N1 Zn 130.9(2) . .
N3 C2 N1 113.6(3) 6_554 .
N3 C2 H2 123.2 6_554 .
N1 C2 H2 123.2 . .
C2 N3 C4 104.8(3) 6 6
C2 N3 Zn 121.0(2) 6 .
C4 N3 Zn 133.8(3) 6 .
C5 C4 N3 108.7(3) . 6_554
C5 C4 H4 125.6 . .
N3 C4 H4 125.6 6_554 .
C4 C5 N1 108.2(3) . .
C4 C5 H5 125.9 . .
N1 C5 H5 125.9 . .
C7 N6 C10 104.6(2) . .
C7 N6 Zn 125.50(19) . .
C10 N6 Zn 128.5(2) . .
N8 C7 N6 113.2(2) 4_455 .
N8 C7 H7 123.4 4_455 .
N6 C7 H7 123.4 . .
C7 N8 C9 105.4(2) 12_454 12_454
C7 N8 Zn 125.58(19) 12_454 .
C9 N8 Zn 128.9(2) 12_454 .
C10 C9 N8 107.6(3) . 4_455
C10 C9 H9 126.2 . .
N8 C9 H9 126.2 4_455 .
C9 C10 N6 109.2(3) . .
C9 C10 H10 125.4 . .
N6 C10 H10 125.4 . .
C12 N11 C12 116.9(7) . 2_565
N11 C12 C13 123.7(6) . .
N11 C12 H12 118.2 . .
C13 C12 H12 118.2 . .
C14 C13 C12 118.7(6) . .
C14 C13 H13 120.7 . .
C12 C13 H13 120.7 . .
C13 C14 C13 118.4(7) . 2_565
C13 C14 H14 120.8 . .
C13 C14 H14 120.8 2_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn N8 1.985(2) .
Zn N6 1.992(2) .
Zn N1 1.992(3) .
Zn N3 2.009(3) .
N1 C2 1.330(4) .
N1 C5 1.367(4) .
C2 N3 1.320(5) 6_554
C2 H2 0.9300 .
N3 C2 1.320(5) 6
N3 C4 1.363(4) 6
C4 C5 1.353(5) .
C4 N3 1.363(4) 6_554
C4 H4 0.9300 .
C5 H5 0.9300 .
N6 C7 1.333(4) .
N6 C10 1.367(4) .
C7 N8 1.332(4) 4_455
C7 H7 0.9300 .
N8 C7 1.332(4) 12_454
N8 C9 1.370(4) 12_454
C9 C10 1.361(4) .
C9 N8 1.370(4) 4_455
C9 H9 0.9300 .
C10 H10 0.9300 .
N11 C12 1.288(7) .
N11 C12 1.288(7) 2_565
C12 C13 1.341(10) .
C12 H12 0.9300 .
C13 C14 1.335(9) .
C13 H13 0.9300 .
C14 C13 1.335(9) 2_565
C14 H14 0.9300 .
