#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:25:23 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178949 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/78/4117850.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_4117850
loop_
_publ_author_name
'Thomas M. McDonald'
'Woo Ram Lee'
'Jarad A. Mason'
'Brian M. Wiers'
'Chang Seop Hong'
'Jeffrey R. Long'
_publ_section_title
;
 Capture of Carbon Dioxide from Air and Flue Gas in the
 Alkylamine-Appended Metal-Organic Framework mmen-Mg2(dobpdc)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7056
_journal_page_last               7065
_journal_paper_doi               10.1021/ja300034j
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C12 H14 N O4 Zn'
_chemical_formula_weight         301.61
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           154
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   21.698(3)
_cell_length_b                   21.698(3)
_cell_length_c                   6.8690(14)
_cell_measurement_reflns_used    24618
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.39
_cell_measurement_theta_min      2.59
_cell_volume                     2800.7(8)
_computing_cell_refinement       HKL2000
_computing_data_collection       'PAL ADSC Quantum-210'
_computing_data_reduction        HKL2000
_computing_molecular_graphics    WingX
_computing_publication_material  WingX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'Pt coated Si double crystal'
_diffrn_radiation_source         'bending magnet beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.85000
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13927
_diffrn_reflns_theta_full        30.39
_diffrn_reflns_theta_max         30.39
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    1.319
_exptl_absorpt_correction_T_max  0.7478
_exptl_absorpt_correction_T_min  0.6273
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   HKL2000-Scalepack
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.46(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2941
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.814
_refine_ls_shift/su_mean         0.049
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0904P)²+0.9620P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                2737
_reflns_number_total             2941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja300034j_si_002.cif
_cod_data_source_block           zndobpdc
_cod_database_code               4117850
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'
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
Zn1 Zn 0.60639(3) 0.27947(2) 1.15793(6) 0.02684(18) Uani 1 1 d .
O1 O 0.6490(2) 0.23825(19) 0.9690(4) 0.0322(7) Uani 1 1 d .
O2 O 0.64993(17) 0.36372(16) 0.9446(4) 0.0284(7) Uani 1 1 d .
O3 O 0.58207(17) 0.20738(15) 1.3738(4) 0.0303(7) Uani 1 1 d .
C1 C 0.6138(3) 0.1744(3) 0.8787(6) 0.0298(11) Uani 1 1 d .
C2 C 0.5709(3) 0.4060(2) 1.0143(6) 0.0279(10) Uani 1 1 d .
C3 C 0.5356(3) 0.4398(3) 0.9362(7) 0.0325(11) Uani 1 1 d .
H3 H 0.5428 0.4530 0.8027 0.039 Uiso 1 1 calc R
C4 C 0.4906(3) 0.4551(3) 1.0438(7) 0.0337(11) Uani 1 1 d .
C5 C 0.5638(3) 0.0465(2) 0.9089(6) 0.0338(12) Uani 1 1 d .
H5 H 0.5538 0.0067 0.9881 0.041 Uiso 1 1 calc R
C6 C 0.5962(3) 0.1132(3) 0.9911(6) 0.0344(11) Uani 1 1 d .
H6 H 0.6070 0.1182 1.1262 0.041 Uiso 1 1 calc R
C7 C 0.6179(3) 0.3950(2) 0.8814(7) 0.0310(11) Uani 1 1 d .
O1S O 0.50364(18) 0.2277(2) 1.0379(5) 0.0426(8) Uani 1 1 d .
C1S C 0.4926(3) 0.2359(3) 0.8694(8) 0.0510(15) Uani 1 1 d D
H1S H 0.5327 0.2584 0.7854 0.061 Uiso 1 1 calc R
N1S N 0.4291(3) 0.2159(4) 0.7923(8) 0.095(3) Uani 1 1 d D
C2S C 0.3652(5) 0.1891(7) 0.9245(15) 0.137(5) Uani 1 1 d D
H2S1 H 0.3701 0.1616 1.0325 0.164 Uiso 1 1 calc R
H2S2 H 0.3218 0.1566 0.8504 0.164 Uiso 1 1 calc R
C3S C 0.3569(7) 0.2517(9) 1.011(3) 0.243(12) Uani 1 1 d D
H3S1 H 0.4041 0.2928 1.0362 0.365 Uiso 1 1 calc R
H3S2 H 0.3300 0.2362 1.1332 0.365 Uiso 1 1 calc R
H3S3 H 0.3314 0.2650 0.9179 0.365 Uiso 1 1 calc R
C4S C 0.4276(7) 0.2267(8) 0.5793(13) 0.177(7) Uani 1 1 d D
H4S1 H 0.4762 0.2609 0.5334 0.212 Uiso 1 1 calc R
H4S2 H 0.3967 0.2471 0.5515 0.212 Uiso 1 1 calc R
C5S C 0.3996(10) 0.1560(12) 0.470(2) 0.64(5) Uani 1 1 d D
H5S1 H 0.3644 0.1170 0.5511 0.955 Uiso 1 1 calc R
H5S2 H 0.4393 0.1478 0.4419 0.955 Uiso 1 1 calc R
H5S3 H 0.3774 0.1579 0.3480 0.955 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'
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
O3 Zn1 O1 98.99(14) . 3_665
O3 Zn1 O1 97.30(13) . .
O1 Zn1 O1 160.66(13) 3_665 .
O3 Zn1 O1S 94.46(13) . .
O1 Zn1 O1S 92.80(14) 3_665 .
O1 Zn1 O1S 96.26(14) . .
O3 Zn1 O2 170.65(13) . .
O1 Zn1 O2 81.61(12) 3_665 .
O1 Zn1 O2 80.63(12) . .
O1S Zn1 O2 94.83(13) . .
O3 Zn1 O2 92.26(12) . 3_665
O1 Zn1 O2 79.67(12) 3_665 3_665
O1 Zn1 O2 89.37(13) . 3_665
O1S Zn1 O2 170.62(14) . 3_665
O2 Zn1 O2 78.63(3) . 3_665
O3 Zn1 Zn1 85.11(8) . 3_665
O1 Zn1 Zn1 39.56(9) 3_665 3_665
O1 Zn1 Zn1 132.61(11) . 3_665
O1S Zn1 Zn1 130.89(11) . 3_665
O2 Zn1 Zn1 89.60(8) . 3_665
O2 Zn1 Zn1 43.29(8) 3_665 3_665
O3 Zn1 Zn1 130.14(10) . 2_654
O1 Zn1 Zn1 121.47(10) 3_665 2_654
O1 Zn1 Zn1 39.22(10) . 2_654
O1S Zn1 Zn1 109.94(9) . 2_654
O2 Zn1 Zn1 44.64(9) . 2_654
O2 Zn1 Zn1 70.11(8) 3_665 2_654
Zn1 Zn1 Zn1 107.18(2) 3_665 2_654
C1 O1 Zn1 121.3(3) . 2_654
C1 O1 Zn1 126.3(3) . .
Zn1 O1 Zn1 101.23(14) 2_654 .
C7 O2 Zn1 124.2(3) . .
C7 O2 Zn1 136.9(3) . 2_654
Zn1 O2 Zn1 92.07(12) . 2_654
C7 O3 Zn1 124.5(3) 2_655 .
O1 C1 C2 124.5(4) . 2_654
O1 C1 C6 117.5(4) . .
C2 C1 C6 118.0(4) 2_654 .
C3 C2 C1 118.8(4) . 3_665
C3 C2 C7 116.7(4) . .
C1 C2 C7 124.4(4) 3_665 .
C4 C3 C2 123.6(4) . .
C3 C4 C5 116.3(4) . 3_665
C3 C4 C4 121.6(5) . 4_557
C5 C4 C4 122.1(5) 3_665 4_557
C6 C5 C4 121.9(4) . 2_654
C5 C6 C1 121.4(4) . .
O2 C7 O3 122.4(4) . 3_664
O2 C7 C2 118.9(4) . .
O3 C7 C2 118.7(4) 3_664 .
C1S O1S Zn1 122.1(4) . .
O1S C1S N1S 125.4(6) . .
C1S N1S C4S 116.2(7) . .
C1S N1S C2S 119.2(6) . .
C4S N1S C2S 124.5(7) . .
N1S C2S C3S 112.0(11) . .
N1S C4S C5S 110.6(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O3 2.024(3) .
Zn1 O1 2.027(4) 3_665
Zn1 O1 2.041(3) .
Zn1 O1S 2.100(3) .
Zn1 O2 2.157(3) .
Zn1 O2 2.211(3) 3_665
Zn1 Zn1 3.1443(7) 3_665
Zn1 Zn1 3.1443(7) 2_654
O1 C1 1.352(6) .
O1 Zn1 2.027(4) 2_654
O2 C7 1.266(6) .
O2 Zn1 2.211(3) 2_654
O3 C7 1.275(6) 2_655
C1 C2 1.408(6) 2_654
C1 C6 1.414(7) .
C2 C3 1.406(7) .
C2 C1 1.408(6) 3_665
C2 C7 1.475(7) .
C3 C4 1.390(7) .
C4 C5 1.409(6) 3_665
C4 C4 1.464(9) 4_557
C5 C6 1.374(7) .
C5 C4 1.409(6) 2_654
C7 O3 1.275(6) 3_664
O1S C1S 1.212(6) .
C1S N1S 1.331(7) .
N1S C4S 1.485(9) .
N1S C2S 1.509(10) .
C2S C3S 1.573(14) .
C4S C5S 1.535(19) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.333 0.333 -0.170 1160.8 289.4
