#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:51:43 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179767 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/63/7006396.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_7006396
loop_
_publ_author_name
'Dietzel, Pascal D. C.'
'Blom, Richard'
'Fjellvåg, Helmer'
_publ_section_title
;
 Increased dimensionalities of zinc-diphenic acid coordination polymers
 by simultaneous or subsequent addition of neutral bridging ligands.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              586
_journal_page_last               593
_journal_paper_doi               10.1039/b509746k
_journal_year                    2006
_chemical_formula_moiety         'C17 H14 N O4 Zn'
_chemical_formula_sum            'C17 H14 N O4 Zn'
_chemical_formula_weight         361.66
_chemical_name_systematic
;
Triethylenediamminzin(II) 2,2'-biphenyldicarboxylate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 109.421(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2726(17)
_cell_length_b                   22.632(5)
_cell_length_c                   9.378(2)
_cell_measurement_reflns_used    712
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.6225
_cell_measurement_theta_min      2.923
_cell_volume                     1455.7(6)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'Apex2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'DIAMOND 3.0b (Crystal Impact, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_diffrn_measurement_method       'omega scan'
_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  0.0871
_diffrn_reflns_av_sigmaI/netI    0.1313
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6187
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.707
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.565267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R. H. (1995) Acta Cryst. A51, 33-38.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.002
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.314
_refine_ls_extinction_coef       0.034(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0553
_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)+(0.0860P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                970
_reflns_number_total             1766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b509746k.txt
_cod_data_source_block           pd67ref
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7006396
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.33273(12) 0.0000 0.35454(9) 0.0304(4) Uani 1 2 d S . .
O1 O 0.2261(5) 0.06356(15) 0.4611(4) 0.0422(10) Uani 1 1 d . . .
O2 O 0.5201(6) -0.06207(18) 0.3255(4) 0.0521(11) Uani 1 1 d . . .
N1 N 0.1289(8) 0.0000 0.1348(6) 0.0291(14) Uani 1 2 d S . .
C1 C 0.3153(8) 0.0810(2) 0.5928(6) 0.0331(12) Uani 1 1 d . . .
C2 C 0.2214(7) 0.1264(2) 0.6629(5) 0.0296(12) Uani 1 1 d . . .
C3 C 0.0466(7) 0.1551(2) 0.5844(5) 0.0296(12) Uani 1 1 d . . .
C4 C -0.0358(8) 0.1930(2) 0.6635(6) 0.0407(14) Uani 1 1 d . . .
H4 H -0.1523 0.2119 0.6116 0.049 Uiso 1 1 calc R . .
C5 C 0.0498(8) 0.2032(2) 0.8161(6) 0.0428(14) Uani 1 1 d . . .
H5 H -0.0098 0.2280 0.8667 0.051 Uiso 1 1 calc R . .
C6 C 0.2248(8) 0.1762(2) 0.8933(6) 0.0397(14) Uani 1 1 d . . .
H6 H 0.2861 0.1835 0.9958 0.048 Uiso 1 1 calc R . .
C7 C 0.3080(8) 0.1385(2) 0.8166(5) 0.0335(12) Uani 1 1 d . . .
H7 H 0.4259 0.1204 0.8692 0.040 Uiso 1 1 calc R . .
C8A C -0.074(2) 0.0000 0.1426(19) 0.062(6) Uani 0.50 2 d SP . .
H8A1 H -0.0913 0.0347 0.1976 0.074 Uiso 0.25 1 calc PR . .
H8A2 H -0.0913 -0.0347 0.1976 0.074 Uiso 0.25 1 calc PR . .
C8B C 0.226(3) 0.0000 0.013(2) 0.076(7) Uani 0.50 2 d SP . .
H8B1 H 0.3082 0.0347 0.0242 0.091 Uiso 0.25 1 calc PR . .
H8B2 H 0.3082 -0.0347 0.0242 0.091 Uiso 0.25 1 calc PR . .
C9A C 0.148(3) 0.0515(7) 0.0522(15) 0.075(5) Uani 0.50 1 d P . .
H9A1 H 0.2750 0.0517 0.0400 0.090 Uiso 0.50 1 calc PR . .
H9A2 H 0.1369 0.0866 0.1082 0.090 Uiso 0.50 1 calc PR . .
C9B C 0.015(3) 0.0524(8) 0.1073(16) 0.104(8) Uani 0.50 1 d P . .
H9B1 H 0.0992 0.0862 0.1137 0.125 Uiso 0.50 1 calc PR . .
H9B2 H -0.0453 0.0567 0.1847 0.125 Uiso 0.50 1 calc PR . .
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'
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
O2 Zn1 O2 87.2(2) 6 . y
O2 Zn1 O1 87.67(16) 6 . y
O2 Zn1 O1 158.30(15) . . y
O2 Zn1 O1 158.30(15) 6 6 y
O2 Zn1 O1 87.67(16) . 6 y
O1 Zn1 O1 89.4(2) . 6 y
O2 Zn1 N1 98.86(15) 6 . y
O2 Zn1 N1 98.86(15) . . y
O1 Zn1 N1 102.76(15) . . y
O1 Zn1 N1 102.76(15) 6 . y
O2 Zn1 Zn1 75.20(11) 6 5_656 ?
O2 Zn1 Zn1 75.20(11) . 5_656 ?
O1 Zn1 Zn1 83.10(10) . 5_656 ?
O1 Zn1 Zn1 83.10(10) 6 5_656 ?
N1 Zn1 Zn1 171.63(17) . 5_656 ?
C1 O1 Zn1 123.2(3) . . ?
C1 O2 Zn1 134.0(3) 5_656 . ?
C9B N1 C9B 113(2) 6 . ?
C9B N1 C9A 51.4(10) 6 6 ?
C9B N1 C9A 137.4(8) . 6 ?
C9B N1 C9A 137.4(8) 6 . ?
C9B N1 C9A 51.4(10) . . ?
C9A N1 C9A 109.1(17) 6 . ?
C9B N1 C8A 59.0(11) 6 . ?
C9B N1 C8A 59.0(11) . . ?
C9A N1 C8A 107.4(9) 6 . ?
C9A N1 C8A 107.4(9) . . ?
C9B N1 C8B 104.5(10) 6 . ?
C9B N1 C8B 104.5(10) . . ?
C9A N1 C8B 56.3(9) 6 . ?
C9A N1 C8B 56.3(9) . . ?
C8A N1 C8B 137.9(10) . . ?
C9B N1 Zn1 110.9(6) 6 . ?
C9B N1 Zn1 110.9(6) . . ?
C9A N1 Zn1 111.6(6) 6 . ?
C9A N1 Zn1 111.6(6) . . ?
C8A N1 Zn1 109.7(7) . . ?
C8B N1 Zn1 112.5(8) . . ?
O1 C1 O2 124.5(5) . 5_656 ?
O1 C1 C2 119.1(5) . . ?
O2 C1 C2 116.4(4) 5_656 . ?
C7 C2 C3 118.2(4) . . ?
C7 C2 C1 118.2(4) . . ?
C3 C2 C1 123.6(4) . . ?
C4 C3 C2 118.8(4) . . ?
C4 C3 C3 116.0(4) . 2_556 ?
C2 C3 C3 124.6(5) . 2_556 ?
C5 C4 C3 122.0(5) . . ?
C5 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
C4 C5 C6 119.4(5) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C7 C6 C5 119.2(5) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C6 C7 C2 122.3(5) . . ?
C6 C7 H7 118.8 . . ?
C2 C7 H7 118.8 . . ?
N1 C8A C8B 111.8(13) . 5 ?
N1 C8A H8A1 109.3 . . ?
C8B C8A H8A1 109.3 5 . ?
N1 C8A H8A2 109.3 . . ?
C8B C8A H8A2 109.3 5 . ?
H8A1 C8A H8A2 107.9 . . ?
C8A C8B N1 110.3(14) 5 . ?
C8A C8B H8B1 109.6 5 . ?
N1 C8B H8B1 109.6 . . ?
C8A C8B H8B2 109.6 5 . ?
N1 C8B H8B2 109.6 . . ?
H8B1 C8B H8B2 108.1 . . ?
N1 C9A C9B 110.4(11) . 2 ?
N1 C9A H9A1 109.6 . . ?
C9B C9A H9A1 109.6 2 . ?
N1 C9A H9A2 109.6 . . ?
C9B C9A H9A2 109.6 2 . ?
H9A1 C9A H9A2 108.1 . . ?
N1 C9B C9A 111.9(11) . 2 ?
N1 C9B H9B1 109.2 . . ?
C9A C9B H9B1 109.2 2 . ?
N1 C9B H9B2 109.2 . . ?
C9A C9B H9B2 109.2 2 . ?
H9B1 C9B H9B2 107.9 . . ?
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 O2 2.037(4) 6 y
Zn1 O2 2.037(4) . y
Zn1 O1 2.046(3) . y
Zn1 O1 2.046(3) 6 y
Zn1 N1 2.101(5) . y
Zn1 Zn1 2.9914(16) 5_656 ?
O1 C1 1.253(6) . ?
O2 C1 1.263(6) 5_656 ?
N1 C9B 1.420(13) 6 ?
N1 C9B 1.420(13) . ?
N1 C9A 1.431(13) 6 ?
N1 C9A 1.431(13) . ?
N1 C8A 1.501(18) . ?
N1 C8B 1.534(19) . ?
C1 O2 1.263(6) 5_656 ?
C1 C2 1.501(7) . ?
C2 C7 1.394(6) . ?
C2 C3 1.399(7) . ?
C3 C4 1.392(7) . ?
C3 C3 1.501(9) 2_556 ?
C4 C5 1.377(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.380(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.379(7) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8A C8B 1.51(2) 5 ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C8B C8A 1.51(2) 5 ?
C8B H8B1 0.9700 . ?
C8B H8B2 0.9700 . ?
C9A C9B 1.568(16) 2 ?
C9A H9A1 0.9700 . ?
C9A H9A2 0.9700 . ?
C9B C9A 1.568(16) 2 ?
C9B H9B1 0.9700 . ?
C9B H9B2 0.9700 . ?
