#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:56:56 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179605 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/69/4506903.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_4506903
loop_
_publ_author_name
'Manos, Manolis J.'
'Moushi, Eleni E.'
'Papaefstathiou, Giannis S.'
'Tasiopoulos, Anastasios J.'
_publ_section_title
;
 New Zn2+Metal Organic Frameworks with Unique Network Topologies from the
 Combination of Trimesic Acid and Amino-Alcohols
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5471
_journal_paper_doi               10.1021/cg301047w
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C27 H9 O18 Zn3, 2(C6 H15 N), C2 H8 N'
_chemical_formula_sum            'C41 H47 N3 O18 Zn3'
_chemical_formula_weight         1065.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           67
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2'
_symmetry_space_group_name_H-M   'C m m a'
_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            4
_cell_length_a                   14.2247(5)
_cell_length_b                   32.481(3)
_cell_length_c                   15.5954(9)
_cell_measurement_reflns_used    7440
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.2340
_cell_measurement_theta_min      3.0433
_cell_volume                     7205.6(8)
_computing_cell_refinement       'CrysAlis RED'
_computing_data_collection       'CrysAlis CCD'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics
;
 DIAMOND (Brandenburg, 2006)
 MERCURY (Bruno et al. 2002)
;
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4223
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22335
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.489
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3355
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0884
_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)+(0.1902P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2662
_refine_ls_wR_factor_ref         0.2758
_reflns_number_gt                2090
_reflns_number_total             3355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301047w_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        7205.7(8)
_cod_database_code               4506903
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z'
'-x, y+1/2, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1, -z'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z'
'x, -y-1/2, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z'
'-x+1/2, y+1/2, z'
'x+1/2, -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
Zn1 Zn 0.38013(6) 0.2500 0.79726(6) 0.0535(5) Uani 1 2 d S
Zn2 Zn 0.2500 0.0000 0.5000 0.0680(6) Uani 1 4 d S
O1 O 0.2482(4) 0.2500 0.8207(4) 0.0679(18) Uani 1 2 d S
O2 O 0.1796(6) 0.2500 0.6964(5) 0.225(10) Uani 1 2 d S
O3 O 0.4223(4) 0.2500 0.9162(3) 0.0709(19) Uani 1 2 d S
O4 O 0.4224(3) 0.19976(17) 0.7452(4) 0.0819(16) Uani 1 1 d .
O5 O 0.3363(5) 0.03080(19) 0.5676(5) 0.121(3) Uani 1 1 d .
O6 O 0.2491(5) 0.0822(2) 0.6158(5) 0.127(3) Uani 1 1 d .
N1 N 0.0000 0.0695(6) 0.7376(13) 0.194(5) Uani 1 2 d SDU
C1 C 0.0839(5) 0.2500 0.9068(4) 0.044(2) Uani 1 2 d S
H1 H 0.1407 0.2500 0.9364 0.053 Uiso 1 2 calc SR
C2 C 0.0843(5) 0.2500 0.8213(5) 0.052(2) Uani 1 2 d S
C3 C 0.0000 0.2500 0.7761(7) 0.063(4) Uani 1 4 d S
H3 H 0.0000 0.2500 0.7165 0.075 Uiso 1 4 calc SR
C4 C 0.5000 0.2500 1.0479(7) 0.046(3) Uani 1 4 d S
C5 C 0.1780(6) 0.2500 0.7748(6) 0.075(3) Uani 1 2 d S
C6 C 0.5000 0.2500 0.9521(8) 0.058(3) Uani 1 4 d S
C7 C 0.5000 0.0673(3) 0.6083(7) 0.074(3) Uani 1 2 d S
H7 H 0.5000 0.0417 0.5815 0.089 Uiso 1 2 calc SR
C8 C 0.4136(5) 0.0865(2) 0.6283(5) 0.077(2) Uani 1 1 d .
C9 C 0.4161(5) 0.1234(2) 0.6693(5) 0.0684(19) Uani 1 1 d .
H9 H 0.3600 0.1364 0.6837 0.082 Uiso 1 1 calc R
C10 C 0.5000 0.1420(3) 0.6900(5) 0.060(2) Uani 1 2 d S
C11 C 0.5000 0.1832(3) 0.7297(6) 0.063(3) Uani 1 2 d S
C12 C 0.3242(6) 0.0654(3) 0.6023(7) 0.091(3) Uani 1 1 d .
C13 C 0.0763(12) 0.0427(5) 0.7100(11) 0.213(6) Uani 1 1 d DU
H13A H 0.0701 0.0163 0.7374 0.320 Uiso 1 1 calc R
H13B H 0.1355 0.0548 0.7254 0.320 Uiso 1 1 calc R
H13C H 0.0735 0.0392 0.6489 0.320 Uiso 1 1 calc R
C14 C 0.0000 0.1065(7) 0.6065(12) 0.205(5) Uani 1 2 d SDU
H14A H 0.0570 0.0932 0.5886 0.308 Uiso 0.50 1 calc PR
H14B H -0.0040 0.1332 0.5804 0.308 Uiso 0.50 1 calc PR
H14C H -0.0530 0.0902 0.5893 0.308 Uiso 0.50 1 calc PR
C15 C 0.0000 0.1111(6) 0.7025(12) 0.198(5) Uani 1 2 d SDU
C16 C 0.0900(9) 0.1318(5) 0.7299(10) 0.192(5) Uani 1 1 d DU
H16A H 0.0915 0.1339 0.7913 0.288 Uiso 1 1 calc R
H16B H 0.0931 0.1588 0.7051 0.288 Uiso 1 1 calc R
H16C H 0.1427 0.1158 0.7106 0.288 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
O1 Zn1 O4 112.86(16) . .
O1 Zn1 O4 112.86(16) . 12_565
O4 Zn1 O4 116.5(3) . 12_565
O1 Zn1 O3 96.9(3) . .
O4 Zn1 O3 107.81(19) . .
O4 Zn1 O3 107.81(19) 12_565 .
O5 Zn2 O5 99.6(5) 8_546 6_545
O5 Zn2 O5 112.7(5) 8_546 3_556
O5 Zn2 O5 116.6(4) 6_545 3_556
O5 Zn2 O5 116.6(4) 8_546 .
O5 Zn2 O5 112.7(5) 6_545 .
O5 Zn2 O5 99.6(5) 3_556 .
C5 O1 Zn1 133.3(6) . .
C6 O3 Zn1 134.7(6) . .
C11 O4 Zn1 136.4(6) . .
C12 O5 Zn2 128.3(6) . .
C13 N1 C13 96.3(19) 11 .
C13 N1 C15 116.3(13) 11 .
C13 N1 C15 116.3(13) . .
C2 C1 C4 120.9(7) . 13_557
C2 C1 H1 119.6 . .
C4 C1 H1 119.6 13_557 .
C1 C2 C3 120.2(7) . .
C1 C2 C5 118.8(7) . .
C3 C2 C5 121.0(8) . .
C2 C3 C2 119.2(10) . 2
C2 C3 H3 120.4 . .
C2 C3 H3 120.4 2 .
C1 C4 C1 118.7(9) 14_557 13_557
C1 C4 C6 120.6(4) 14_557 .
C1 C4 C6 120.6(4) 13_557 .
O2 C5 O1 124.5(9) . .
O2 C5 C2 119.7(9) . .
O1 C5 C2 115.8(8) . .
O3 C6 O3 126.3(11) 2_655 .
O3 C6 C4 116.8(5) 2_655 .
O3 C6 C4 116.8(5) . .
C8 C7 C8 120.8(10) 11_655 .
C8 C7 H7 119.6 11_655 .
C8 C7 H7 119.6 . .
C9 C8 C7 118.0(8) . .
C9 C8 C12 123.5(7) . .
C7 C8 C12 118.5(8) . .
C8 C9 C10 121.3(7) . .
C8 C9 H9 119.3 . .
C10 C9 H9 119.3 . .
C9 C10 C9 120.4(9) . 11_655
C9 C10 C11 119.8(5) . .
C9 C10 C11 119.8(5) 11_655 .
O4 C11 O4 123.8(10) 11_655 .
O4 C11 C10 118.1(5) 11_655 .
O4 C11 C10 118.1(5) . .
O6 C12 O5 126.4(8) . .
O6 C12 C8 119.6(8) . .
O5 C12 C8 114.0(8) . .
N1 C13 H13A 109.5 . .
N1 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
N1 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C15 C14 H14A 109.5 . .
C15 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C15 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
N1 C15 C14 106.4(18) . .
N1 C15 C16 107.9(12) . .
C14 C15 C16 109.0(12) . .
N1 C15 C16 107.9(12) . 11
C14 C15 C16 109.0(12) . 11
C16 C15 C16 116.2(18) . 11
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.911(6) .
Zn1 O4 1.919(5) .
Zn1 O4 1.919(5) 12_565
Zn1 O3 1.949(5) .
Zn2 O5 1.902(6) 8_546
Zn2 O5 1.902(6) 6_545
Zn2 O5 1.902(6) 3_556
Zn2 O5 1.902(6) .
O1 C5 1.230(11) .
O2 C5 1.222(11) .
O3 C6 1.239(8) .
O4 C11 1.252(6) .
O5 C12 1.260(10) .
O6 C12 1.216(10) .
N1 C13 1.457(5) 11
N1 C13 1.457(5) .
N1 C15 1.456(5) .
C1 C2 1.334(11) .
C1 C4 1.387(8) 13_557
C1 H1 0.9300 .
C2 C3 1.391(9) .
C2 C5 1.516(11) .
C3 C2 1.391(9) 2
C3 H3 0.9300 .
C4 C1 1.387(8) 14_557
C4 C1 1.387(8) 13_557
C4 C6 1.495(16) .
C6 O3 1.239(8) 2_655
C7 C8 1.414(9) 11_655
C7 C8 1.414(9) .
C7 H7 0.9300 .
C8 C9 1.360(10) .
C8 C12 1.500(11) .
C9 C10 1.375(8) .
C9 H9 0.9300 .
C10 C9 1.375(8) 11_655
C10 C11 1.476(14) .
C11 O4 1.251(6) 11_655
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 C15 1.505(5) .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 C16 1.508(5) .
C15 C16 1.508(5) 11
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
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
_platon_squeeze_void_content
1 -0.022 0.000 0.000 1283 168 ' '
2 -0.022 0.250 0.500 474 68 ' '
3 -0.021 0.500 0.000 1283 168 ' '
4 -0.022 0.750 0.500 474 68 ' '
