#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/21/7112149.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_7112149
loop_
_publ_author_name
'In-Hyeok Park'
'Anjana Chanthapally'
'Hyeong-Hwan Lee'
'Hong Sheng Quah'
'Shim Sung Lee'
'Jagadese J. Vittal'
_publ_section_title
;
 Solid-State Conversion of a MOF to a Metal-Organo Polymeric Framework
 (MOPF) via [2+2] Cycloaddition Reaction
;
_journal_name_full               Chem.Commun.
_journal_page_first              3665
_journal_paper_doi               10.1039/C4CC00228H
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C15 H12 N O4.5 Zn'
_chemical_formula_weight         343.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 111.283(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3685(18)
_cell_length_b                   22.092(4)
_cell_length_c                   9.448(2)
_cell_measurement_reflns_used    2387
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.43
_cell_measurement_theta_min      2.49
_cell_volume                     1433.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.1037
_diffrn_reflns_av_sigmaI/netI    0.1002
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12614
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.732
_exptl_absorpt_correction_T_max  0.9032
_exptl_absorpt_correction_T_min  0.3769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0672
_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)+(0.0016P)²+2.9001P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1631
_reflns_number_gt                1895
_reflns_number_total             2810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc00228h.txt
_cod_data_source_block           form2
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C15 H12 N O4.50 Zn'
_cod_database_code               7112149
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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_group
Zn1 Zn 0.59827(11) 0.24389(2) 0.57986(9) 0.0606(3) Uani 1 1 d . .
O1 O 0.4562(8) 0.16381(17) 0.5356(5) 0.0829(15) Uani 1 1 d . .
O2 O 0.7631(9) 0.14426(19) 0.5903(6) 0.0949(18) Uani 1 1 d . .
N1 N 0.3777(7) 0.30531(18) 0.5282(6) 0.0555(13) Uani 1 1 d . .
C1 C 0.2961(9) 0.3209(2) 0.6309(8) 0.0603(17) Uani 1 1 d . .
H1 H 0.3330 0.2992 0.7240 0.072 Uiso 1 1 calc R .
C2 C 0.1612(9) 0.3671(2) 0.6045(7) 0.0547(15) Uani 1 1 d . .
H2 H 0.1071 0.3764 0.6792 0.066 Uiso 1 1 calc R .
C3 C 0.1042(7) 0.4000(2) 0.4708(6) 0.0410(12) Uani 1 1 d . .
C4 C 0.1803(8) 0.3816(2) 0.3615(7) 0.0466(13) Uani 1 1 d . .
H4 H 0.1393 0.4009 0.2651 0.056 Uiso 1 1 calc R .
C5 C 0.3160(9) 0.3351(2) 0.3954(7) 0.0554(15) Uani 1 1 d . .
H5 H 0.3679 0.3238 0.3207 0.066 Uiso 1 1 calc R .
C6 C -0.0208(7) 0.4560(2) 0.4390(6) 0.0345(11) Uani 1 1 d . .
H6 H -0.1353 0.4509 0.3423 0.041 Uiso 1 1 calc R .
C7 C -0.0885(6) 0.48220(19) 0.5650(6) 0.0333(11) Uani 1 1 d . .
H7 H -0.0247 0.4605 0.6636 0.040 Uiso 1 1 calc R .
C8 C -0.3026(6) 0.4882(2) 0.5277(6) 0.0354(11) Uani 1 1 d . .
C9 C -0.4274(6) 0.5089(2) 0.3858(6) 0.0377(12) Uani 1 1 d . .
H9 H -0.3785 0.5150 0.3067 0.045 Uiso 1 1 calc R .
C10 C -0.3782(7) 0.4794(2) 0.6406(6) 0.0373(11) Uani 1 1 d . .
H10 H -0.2958 0.4651 0.7375 0.045 Uiso 1 1 calc R .
C11 C 0.5916(12) 0.1282(3) 0.5504(7) 0.0656(19) Uani 1 1 d . .
C12 C 0.5416(9) 0.0611(2) 0.5232(6) 0.0460(13) Uani 1 1 d . .
C13 C 0.3552(9) 0.0406(2) 0.4931(6) 0.0499(14) Uani 1 1 d . .
H13 H 0.2548 0.0684 0.4886 0.060 Uiso 1 1 calc R .
C14 C 0.6864(9) 0.0208(2) 0.5307(6) 0.0513(14) Uani 1 1 d . .
H14 H 0.8155 0.0349 0.5523 0.062 Uiso 1 1 calc R .
O3 O 0.8463(10) 0.2271(3) 0.2391(8) 0.052(2) Uani 0.563(8) 1 d P 1
O4 O 0.669(5) 0.2516(10) 0.367(3) 0.054(5) Uani 0.563(8) 1 d P 1
C15 C 0.8267(15) 0.2343(4) 0.3647(13) 0.046(3) Uani 0.563(8) 1 d P 1
H15 H 0.9324 0.2266 0.4569 0.056 Uiso 0.563(8) 1 calc PR 1
O3A O 0.7959(13) 0.2825(4) 0.5568(12) 0.059(3) Uani 0.437(8) 1 d P 2
O4A O 0.636(5) 0.2609(15) 0.327(5) 0.070(11) Uani 0.437(8) 1 d P 2
C15A C 0.778(2) 0.2773(7) 0.4165(19) 0.045(4) Uani 0.437(8) 1 d P 2
H15A H 0.8844 0.2873 0.3869 0.054 Uiso 0.437(8) 1 calc PR 2
O1W O 0.973(2) 0.1360(7) 0.4052(18) 0.145(5) Uiso 0.50 1 d P .
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
O3A Zn1 O3 51.0(4) . 4_566
O3A Zn1 O1 141.7(3) . .
O3 Zn1 O1 134.2(2) 4_566 .
O3A Zn1 N1 105.7(3) . .
O3 Zn1 N1 113.5(2) 4_566 .
O1 Zn1 N1 103.0(2) . .
O3A Zn1 O4A 110.8(8) . 4_566
O3 Zn1 O4A 60.1(8) 4_566 4_566
O1 Zn1 O4A 91.9(7) . 4_566
N1 Zn1 O4A 93.8(10) . 4_566
O3A Zn1 O4 52.3(9) . .
O3 Zn1 O4 101.7(9) 4_566 .
O1 Zn1 O4 98.7(8) . .
N1 Zn1 O4 99.0(6) . .
O4A Zn1 O4 161.1(5) 4_566 .
O3A Zn1 C15A 29.7(5) . .
O3 Zn1 C15A 79.9(5) 4_566 .
O1 Zn1 C15A 119.0(4) . .
N1 Zn1 C15A 102.2(4) . .
O4A Zn1 C15A 140.1(8) 4_566 .
O4 Zn1 C15A 22.7(8) . .
O3A Zn1 C11 116.8(3) . .
O3 Zn1 C11 112.1(3) 4_566 .
O1 Zn1 C11 28.2(2) . .
N1 Zn1 C11 130.9(2) . .
O4A Zn1 C11 93.2(8) 4_566 .
O4 Zn1 C11 88.9(6) . .
C15A Zn1 C11 102.8(4) . .
C11 O1 Zn1 101.4(5) . .
C5 N1 C1 117.2(5) . .
C5 N1 Zn1 121.4(4) . .
C1 N1 Zn1 121.3(4) . .
N1 C1 C2 122.3(6) . .
C3 C2 C1 120.8(5) . .
C2 C3 C4 116.8(5) . .
C2 C3 C6 125.0(4) . .
C4 C3 C6 118.0(5) . .
C5 C4 C3 119.4(5) . .
N1 C5 C4 123.4(5) . .
C3 C6 C7 119.6(4) . .
C3 C6 C7 115.5(4) . 3_566
C7 C6 C7 90.3(3) . 3_566
C8 C7 C6 117.2(4) . .
C8 C7 C6 114.7(4) . 3_566
C6 C7 C6 89.7(3) . 3_566
C10 C8 C9 118.4(4) . .
C10 C8 C7 119.5(5) . .
C9 C8 C7 121.7(4) . .
C10 C9 C8 120.7(4) 3_466 .
C8 C10 C9 120.9(5) . 3_466
O2 C11 O1 123.2(6) . .
O2 C11 C12 119.2(6) . .
O1 C11 C12 117.6(7) . .
O2 C11 Zn1 72.8(4) . .
O1 C11 Zn1 50.5(3) . .
C12 C11 Zn1 168.0(5) . .
C14 C12 C13 119.8(5) . .
C14 C12 C11 119.1(6) . .
C13 C12 C11 121.1(5) . .
C12 C13 C14 120.0(5) . 3_656
C12 C14 C13 120.2(5) . 3_656
C15 O3 Zn1 106.4(6) . 4_565
C15 O4 Zn1 120.9(18) . .
O4 C15 O3 119.1(17) . .
C15A O3A Zn1 107.5(9) . .
C15A O4A Zn1 121(2) . 4_565
O4A C15A O3A 120.8(19) . .
O4A C15A Zn1 79.0(17) . .
O3A C15A Zn1 42.8(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O3A 1.768(8) .
Zn1 O3 2.004(7) 4_566
Zn1 O1 2.021(4) .
Zn1 N1 2.036(4) .
Zn1 O4A 2.26(4) 4_566
Zn1 O4 2.26(3) .
Zn1 C15A 2.482(14) .
Zn1 C11 2.569(6) .
O1 C11 1.237(8) .
O2 C11 1.233(8) .
N1 C5 1.341(7) .
N1 C1 1.358(7) .
C1 C2 1.384(7) .
C2 C3 1.384(8) .
C3 C4 1.401(7) .
C3 C6 1.507(6) .
C4 C5 1.388(7) .
C6 C7 1.559(6) .
C6 C7 1.593(6) 3_566
C7 C8 1.492(6) .
C7 C6 1.593(6) 3_566
C8 C10 1.385(7) .
C8 C9 1.399(7) .
C9 C10 1.386(6) 3_466
C10 C9 1.386(6) 3_466
C11 C12 1.526(7) .
C12 C14 1.372(8) .
C12 C13 1.374(8) .
C13 C14 1.393(7) 3_656
C14 C13 1.393(7) 3_656
O3 C15 1.256(12) .
O3 Zn1 2.004(7) 4_565
O4 C15 1.23(3) .
O3A C15A 1.289(18) .
O4A C15A 1.14(5) .
O4A Zn1 2.26(4) 4_565
