#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/30/4503031.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_4503031
loop_
_publ_author_name
'Mulfort, Karen L.'
'Wilson, Thea M.'
'Wasielewski, Michael R.'
'Hupp, Joseph T.'
_publ_contact_author             'Joseph T. Hupp'
_publ_section_title
;
 Framework reduction and alkali-metal doping of a triply catenating
 metal-organic framework enhances and then diminishes H2 uptake.
;
_journal_issue                   1
_journal_name_full
'Langmuir : the ACS journal of surfaces and colloids'
_journal_page_first              503
_journal_page_last               508
_journal_paper_doi               10.1021/la803014k
_journal_volume                  25
_journal_year                    2009
_chemical_formula_sum            'C18.5 H10 N4 O4 Zn'
_chemical_formula_weight         417.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.845(7)
_cell_angle_beta                 72.778(4)
_cell_angle_gamma                88.703(5)
_cell_formula_units_Z            2
_cell_length_a                   7.815(2)
_cell_length_b                   10.746(3)
_cell_length_c                   13.028(5)
_cell_measurement_reflns_used    4437
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.17
_cell_volume                     983.8(5)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_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  0.1098
_diffrn_reflns_av_sigmaI/netI    0.1188
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11429
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_T_max  0.9346
_exptl_absorpt_correction_T_min  0.8658
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.057
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.028
_platon_squeeze_details          ' ?'
_refine_diff_density_max         2.890
_refine_diff_density_min         -2.994
_refine_diff_density_rms         0.289
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.1351
_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)+(0.1250P)²+35.9257P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3601
_refine_ls_wR_factor_ref         0.3686
_reflns_number_gt                3341
_reflns_number_total             4561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            la803014k_si_002.cif
_cod_data_source_block           zn2ndc2dipytz_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C18.50 H10 N4 O4 Zn'
_cod_database_code               4503031
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
C1 C 0.5551(16) 0.6666(12) 0.3146(10) 0.022(2) Uiso 1 1 d .
H1 H 0.5664 0.5809 0.3631 0.026 Uiso 1 1 calc R
H2 H 0.8201 0.6988 0.2507 0.026 Uiso 1 1 d R
C3 C 0.6936(18) 0.8591(14) 0.1643(12) 0.033(3) Uani 1 1 d .
C4 C 0.525(2) 0.9054(15) 0.1715(13) 0.042(4) Uani 1 1 d .
H4 H 0.5108 0.9905 0.1231 0.050 Uiso 1 1 calc R
C5 C 0.3749(19) 0.8221(13) 0.2529(11) 0.029(3) Uiso 1 1 d .
H5 H 0.2583 0.8522 0.2587 0.035 Uiso 1 1 calc R
C6 C 0.8563(19) 0.9381(14) 0.0792(12) 0.032(3) Uiso 1 1 d .
C7 C 0.1776(16) 0.2946(12) 0.5162(10) 0.020(2) Uani 1 1 d .
C8 C 0.2770(15) 0.1712(11) 0.5173(10) 0.019(2) Uani 1 1 d .
C9 C 0.1759(16) 0.0547(12) 0.5415(11) 0.024(3) Uani 1 1 d .
H9 H 0.0486 0.0529 0.5615 0.029 Uiso 1 1 calc R
C10 C 0.2610(16) -0.0598(11) 0.5364(11) 0.024(3) Uani 1 1 d .
H10 H 0.1921 -0.1383 0.5497 0.029 Uiso 1 1 calc R
C11 C 0.4524(15) -0.0587(11) 0.5113(10) 0.018(2) Uani 1 1 d .
C12 C 0.4605(14) 0.1764(10) 0.4897(9) 0.015(2) Uani 1 1 d .
H12 H 0.5286 0.2571 0.4716 0.019 Uiso 1 1 calc R
C13 C -0.0561(16) 0.4712(11) 0.3216(10) 0.019(2) Uani 1 1 d .
C14 C -0.0548(17) 0.4626(12) 0.2078(10) 0.024(3) Uani 1 1 d .
C15 C -0.1570(19) 0.3604(13) 0.2045(11) 0.028(3) Uani 1 1 d .
H15 H -0.2303 0.2982 0.2736 0.034 Uiso 1 1 calc R
C16 C -0.1522(19) 0.3492(13) 0.1022(11) 0.029(3) Uani 1 1 d .
H16 H -0.2164 0.2764 0.1002 0.035 Uiso 1 1 calc R
C17 C -0.0490(17) 0.4484(14) -0.0029(10) 0.026(3) Uani 1 1 d .
C18 C 0.0474(16) 0.5570(12) 0.1110(10) 0.021(2) Uani 1 1 d .
H18 H 0.1166 0.6255 0.1155 0.025 Uiso 1 1 calc R
C2A C 0.714(2) 0.742(2) 0.2424(13) 0.027(5) Uiso 0.99(8) 1 d P
C2B C 0.747(3) 0.801(2) 0.2229(16) 0.001(8) Uiso 0.48(7) 1 d P
N2 N 0.8477(18) 1.0613(13) 0.0186(15) 0.054(4) Uani 1 1 d .
N1A N 0.3910(13) 0.7018(13) 0.3223(9) 0.019(2) Uiso 1 1 d .
N3A N 1.005(3) 0.8730(19) 0.097(3) 0.046(7) Uiso 0.78(9) 1 d P
N1B N 0.408(2) 0.6394(18) 0.3396(13) 0.001(5) Uiso 0.48(4) 1 d P
N3B N 1.006(2) 0.8715(18) 0.051(2) 0.010(8) Uiso 0.48(8) 1 d P
O1 O 0.2694(11) 0.4040(7) 0.4724(7) 0.0190(16) Uani 1 1 d .
O2 O 0.0106(11) 0.2788(8) 0.5560(8) 0.0228(18) Uani 1 1 d .
O3 O 0.0686(11) 0.5422(9) 0.3229(7) 0.0233(18) Uani 1 1 d .
O4 O 0.1821(11) 0.5906(8) 0.5910(6) 0.0188(16) Uani 1 1 d .
Zn1 Zn 0.17074(16) 0.58406(12) 0.43768(10) 0.0106(4) Uani 1 1 d .
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
N1A C1 C2A 126.6(13) . .
N1A C1 C2B 116.6(11) . .
C2A C1 C2B 12.3(8) . .
N1A C1 H1 116.7 . .
C2A C1 H1 116.7 . .
C2B C1 H1 126.1 . .
C2B C3 C2A 24.8(13) . .
C2B C3 C4 132.7(18) . .
C2A C3 C4 120.6(13) . .
C2B C3 C6 100.5(17) . .
C2A C3 C6 118.1(13) . .
C4 C3 C6 121.2(13) . .
C3 C4 C5 117.8(12) . .
C3 C4 H4 121.1 . .
C5 C4 H4 121.1 . .
N1A C5 C4 122.3(12) . .
N1A C5 H5 118.8 . .
C4 C5 H5 118.8 . .
N2 C6 N3B 121.5(15) . .
N2 C6 N3A 129.2(15) . .
N3B C6 N3A 24.9(10) . .
N2 C6 C3 120.3(13) . .
N3B C6 C3 117.1(14) . .
N3A C6 C3 108.8(14) . .
O2 C7 O1 125.4(11) . .
O2 C7 C8 116.9(10) . .
O1 C7 C8 117.6(10) . .
C12 C8 C9 121.2(10) . .
C12 C8 C7 121.0(10) . .
C9 C8 C7 117.6(10) . .
C8 C9 C10 120.2(11) . .
C8 C9 H9 119.9 . .
C10 C9 H9 119.9 . .
C9 C10 C11 120.0(11) . .
C9 C10 H10 120.0 . .
C11 C10 H10 120.0 . .
C11 C11 C12 121.7(13) 2_656 2_656
C11 C11 C10 118.0(12) 2_656 .
C12 C11 C10 120.3(10) 2_656 .
C8 C12 C11 118.8(10) . 2_656
C8 C12 H12 120.6 . .
C11 C12 H12 120.6 2_656 .
O4 C13 O3 123.6(10) 2_566 .
O4 C13 C14 118.7(11) 2_566 .
O3 C13 C14 117.7(11) . .
C18 C14 C15 122.1(11) . .
C18 C14 C13 118.2(11) . .
C15 C14 C13 119.8(11) . .
C16 C15 C14 120.2(12) . .
C16 C15 H15 119.9 . .
C14 C15 H15 119.9 . .
C15 C16 C17 119.7(12) . .
C15 C16 H16 120.1 . .
C17 C16 H16 120.1 . .
C17 C17 C18 120.0(14) 2_565 2_565
C17 C17 C16 118.8(13) 2_565 .
C18 C17 C16 121.2(11) 2_565 .
C14 C18 C17 119.1(11) . 2_565
C14 C18 H18 120.5 . .
C17 C18 H18 120.5 2_565 .
C2B C2A C3 42(2) . .
C2B C2A C1 139(3) . .
C3 C2A C1 115.3(12) . .
C2B C2A H2 99.4 . .
C3 C2A H2 130.7 . .
C1 C2A H2 113.6 . .
C2A C2B C3 113(3) . .
C2A C2B C1 28.3(19) . .
C3 C2B C1 102.1(16) . .
C2A C2B H2 50.3 . .
C3 C2B H2 144.9 . .
C1 C2B H2 74.7 . .
N3B N2 C6 118.3(15) 2_775 .
N3B N2 N3A 21.7(10) 2_775 2_775
C6 N2 N3A 119.6(14) . 2_775
N1B N1A C1 58.2(17) . .
N1B N1A C5 160(2) . .
C1 N1A C5 116.7(11) . .
N1B N1A Zn1 67.9(16) . .
C1 N1A Zn1 122.2(10) . .
C5 N1A Zn1 121.1(9) . .
N3B N3A C6 77(3) . .
N3B N3A N2 53(3) . 2_775
C6 N3A N2 102.4(19) . 2_775
N1A N1B Zn1 93.3(18) . .
N3A N3B N2 105(3) . 2_775
N3A N3B C6 78(3) . .
N2 N3B C6 118.4(16) 2_775 .
C7 O1 Zn1 125.8(8) . .
C7 O2 Zn1 129.4(8) . 2_566
C13 O3 Zn1 139.9(8) . .
C13 O4 Zn1 117.2(7) 2_566 .
N1B Zn1 O2 118.6(6) . 2_566
N1B Zn1 O1 82.7(6) . .
O2 Zn1 O1 158.6(3) 2_566 .
N1B Zn1 N1A 18.8(5) . .
O2 Zn1 N1A 99.8(4) 2_566 .
O1 Zn1 N1A 101.5(4) . .
N1B Zn1 O4 103.8(5) . .
O2 Zn1 O4 86.2(3) 2_566 .
O1 Zn1 O4 89.4(3) . .
N1A Zn1 O4 103.6(4) . .
N1B Zn1 O3 97.2(5) . .
O2 Zn1 O3 87.2(4) 2_566 .
O1 Zn1 O3 89.5(3) . .
N1A Zn1 O3 97.4(4) . .
O4 Zn1 O3 158.7(3) . .
N1B Zn1 Zn1 159.4(5) . 2_566
O2 Zn1 Zn1 78.3(2) 2_566 2_566
O1 Zn1 Zn1 80.7(2) . 2_566
N1A Zn1 Zn1 167.9(3) . 2_566
O4 Zn1 Zn1 88.2(2) . 2_566
O3 Zn1 Zn1 70.6(2) . 2_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1A 1.313(16) .
C1 C2A 1.39(2) .
C1 C2B 1.91(3) .
C1 H1 0.9500 .
C3 C2B 1.00(2) .
C3 C2A 1.37(2) .
C3 C4 1.387(19) .
C3 C6 1.471(18) .
C4 C5 1.410(19) .
C4 H4 0.9500 .
C5 N1A 1.340(18) .
C5 H5 0.9500 .
C6 N2 1.312(19) .
C6 N3B 1.37(2) .
C6 N3A 1.38(2) .
C7 O2 1.246(14) .
C7 O1 1.256(14) .
C7 C8 1.520(15) .
C8 C12 1.369(15) .
C8 C9 1.389(17) .
C9 C10 1.396(16) .
C9 H9 0.9500 .
C10 C11 1.433(16) .
C10 H10 0.9500 .
C11 C11 1.38(2) 2_656
C11 C12 1.425(15) 2_656
C12 C11 1.425(15) 2_656
C12 H12 0.9500 .
C13 O4 1.255(14) 2_566
C13 O3 1.258(15) .
C13 C14 1.513(16) .
C14 C18 1.363(17) .
C14 C15 1.392(18) .
C15 C16 1.366(17) .
C15 H15 0.9500 .
C16 C17 1.445(18) .
C16 H16 0.9500 .
C17 C17 1.40(3) 2_565
C17 C18 1.424(16) 2_565
C18 C17 1.424(16) 2_565
C18 H18 0.9500 .
C2A C2B 0.627(19) .
C2A H2 0.9556 .
C2B H2 1.2249 .
N2 N3B 1.29(2) 2_775
N2 N3A 1.55(3) 2_775
N1A N1B 0.658(15) .
N1A Zn1 2.035(10) .
N3A N3B 0.59(2) .
N3A N2 1.55(3) 2_775
N1B Zn1 1.889(15) .
N3B N2 1.29(2) 2_775
O1 Zn1 2.026(7) .
O2 Zn1 2.025(8) 2_566
O3 Zn1 2.059(8) .
O4 C13 1.255(14) 2_566
O4 Zn1 2.049(7) .
Zn1 O2 2.025(8) 2_566
Zn1 Zn1 2.958(2) 2_566
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 0.500 0.500 0.000 265.1 76.3
