#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:45:29 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178962 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/91/4119105.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4119105
loop_
_publ_author_name
'Dincǎ, Mircea'
'Long, Jeffrey R.'
_publ_section_title
;
 Strong H2Binding and Selective Gas Adsorption within the Microporous
 Coordination Solid Mg3(O2C-C10H6-CO2)3
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9376
_journal_page_last               9377
_journal_paper_doi               10.1021/ja0523082
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C44 H38 N2 O17 Zn3'
_chemical_formula_weight         1062.87
_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                112.33(5)
_cell_angle_beta                 97.31(6)
_cell_angle_gamma                106.79(4)
_cell_formula_units_Z            1
_cell_length_a                   10.327(3)
_cell_length_b                   11.067(6)
_cell_length_c                   11.692(10)
_cell_measurement_reflns_used    7576
_cell_measurement_temperature    132(2)
_cell_measurement_theta_max      52.601
_cell_measurement_theta_min      4.956
_cell_volume                     1140.2(14)
_computing_cell_refinement
;
  SMART (Siemens, 1995), SAINT (Siemens, 1995)
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
;
  SAINT (Siemens, 1995), XPREP (Siemens, 1995)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      132(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       APEX
_diffrn_measurement_method       'omega scans with profile analysis'
_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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7576
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    1.640
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.723395
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             542
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0364
_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)+(0.0626P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                3716
_reflns_number_total             4555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0523082sup2.cif
_cod_data_source_block           md27a
_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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1140.2(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4119105
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
Zn1 Zn 0.16664(3) -0.16711(3) 0.13998(3) 0.01837(11) Uani 1 1 d .
Zn2 Zn 0.0000 0.0000 0.0000 0.01653(12) Uani 1 2 d S
O1 O 0.0065(2) -0.19155(18) -0.10729(18) 0.0228(4) Uani 1 1 d .
O2 O 0.1810(2) -0.2494(2) -0.03622(18) 0.0265(4) Uani 1 1 d .
O3 O 0.2864(2) 0.02213(18) 0.26416(18) 0.0247(4) Uani 1 1 d .
O4 O 0.2087(2) 0.07819(19) 0.11192(17) 0.0227(4) Uani 1 1 d .
O5 O -0.0863(2) -0.07771(19) 0.12441(18) 0.0219(4) Uani 1 1 d .
O6 O -0.0271(2) -0.2532(2) 0.1346(2) 0.0276(5) Uani 1 1 d .
O7 O 0.2438(2) -0.2720(2) 0.2191(2) 0.0353(5) Uani 1 1 d .
O8 O 0.4974(2) 0.8388(2) 0.3649(2) 0.0355(5) Uani 1 1 d .
O9 O -0.4691(7) 0.0430(6) 0.0638(6) 0.0660(16) Uiso 0.50 1 d P
N1 N 0.7135(3) 0.9937(3) 0.3983(3) 0.0467(8) Uani 1 1 d .
C1 C 0.0895(3) -0.2553(3) -0.1247(2) 0.0197(6) Uani 1 1 d .
C2 C 0.0782(3) -0.3504(3) -0.2604(2) 0.0194(5) Uani 1 1 d .
C3 C -0.0317(3) -0.3753(3) -0.3563(3) 0.0209(6) Uani 1 1 d .
H3 H -0.0952 -0.3309 -0.3360 0.025 Uiso 1 1 calc R
C4 C -0.0503(3) -0.4676(3) -0.4860(3) 0.0205(5) Uani 1 1 d .
C5 C -0.1626(3) -0.4957(3) -0.5864(3) 0.0260(6) Uani 1 1 d .
H5 H -0.2281 -0.4537 -0.5680 0.031 Uiso 1 1 calc R
C6 C -0.1766(3) -0.5842(3) -0.7108(3) 0.0244(6) Uani 1 1 d .
H6 H -0.2507 -0.6011 -0.7762 0.029 Uiso 1 1 calc R
C7 C 0.2792(3) 0.1121(3) 0.2217(3) 0.0202(6) Uani 1 1 d .
C8 C 0.3608(3) 0.2642(3) 0.3111(2) 0.0194(5) Uani 1 1 d .
C9 C 0.3666(3) 0.3673(3) 0.2651(3) 0.0234(6) Uani 1 1 d .
H9 H 0.3225 0.3398 0.1800 0.028 Uiso 1 1 calc R
C10 C 0.4369(3) 0.5063(3) 0.3458(3) 0.0224(6) Uani 1 1 d .
H10 H 0.4419 0.5727 0.3145 0.027 Uiso 1 1 calc R
C11 C 0.4267(3) 0.3045(3) 0.4365(2) 0.0198(6) Uani 1 1 d .
H11 H 0.4249 0.2364 0.4651 0.024 Uiso 1 1 calc R
C12 C 0.4976(3) 0.4489(3) 0.5233(2) 0.0182(5) Uani 1 1 d .
C13 C -0.1174(3) -0.2005(3) 0.1148(3) 0.0220(6) Uani 1 1 d .
C14 C -0.2685(3) -0.2946(3) 0.0780(3) 0.0219(6) Uani 1 1 d .
C15 C -0.3762(3) -0.2407(3) 0.0657(3) 0.0235(6) Uani 1 1 d .
H15 H -0.3525 -0.1460 0.0858 0.028 Uiso 1 1 calc R
C16 C -0.5146(3) -0.3273(3) 0.0247(3) 0.0246(6) Uani 1 1 d .
H16 H -0.5840 -0.2906 0.0169 0.029 Uiso 1 1 calc R
C17 C -0.5537(3) -0.4727(3) -0.0064(3) 0.0216(6) Uani 1 1 d .
C18 C -0.6960(3) -0.5654(3) -0.0500(3) 0.0232(6) Uani 1 1 d .
H18 H -0.7668 -0.5309 -0.0599 0.028 Uiso 1 1 calc R
C19 C 0.1603(4) -0.3948(3) 0.2274(4) 0.0415(9) Uani 1 1 d .
H19C H 0.1931 -0.3879 0.3110 0.062 Uiso 1 1 calc R
H19B H 0.1679 -0.4763 0.1635 0.062 Uiso 1 1 calc R
H19A H 0.0641 -0.4025 0.2132 0.062 Uiso 1 1 calc R
C20 C 0.5750(4) 0.9490(3) 0.3686(3) 0.0393(8) Uani 1 1 d .
H20 H 0.5328 1.0051 0.3491 0.047 Uiso 1 1 calc R
C21 C 0.7866(4) 0.9093(5) 0.4248(4) 0.0591(11) Uani 1 1 d .
H21C H 0.8629 0.9129 0.3856 0.089 Uiso 1 1 calc R
H21B H 0.7227 0.8138 0.3906 0.089 Uiso 1 1 calc R
H21A H 0.8225 0.9454 0.5159 0.089 Uiso 1 1 calc R
C22 C 0.8003(7) 1.1238(5) 0.3990(7) 0.107(2) Uani 1 1 d .
H22C H 0.8661 1.1831 0.4818 0.161 Uiso 1 1 calc R
H22B H 0.7417 1.1712 0.3809 0.161 Uiso 1 1 calc R
H22A H 0.8504 1.1029 0.3348 0.161 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
O6 Zn1 O3 123.26(11) . .
O6 Zn1 O2 106.54(11) . .
O3 Zn1 O2 122.54(10) . .
O6 Zn1 O7 96.67(9) . .
O3 Zn1 O7 98.27(11) . .
O2 Zn1 O7 102.84(11) . .
O1 Zn2 O1 180.00(15) . 2
O1 Zn2 O4 86.95(10) . 2
O1 Zn2 O4 93.05(10) 2 2
O1 Zn2 O4 93.05(10) . .
O1 Zn2 O4 86.95(10) 2 .
O4 Zn2 O4 180.00(12) 2 .
O1 Zn2 O5 90.21(9) . 2
O1 Zn2 O5 89.79(9) 2 2
O4 Zn2 O5 93.91(9) 2 2
O4 Zn2 O5 86.09(9) . 2
O1 Zn2 O5 89.79(9) . .
O1 Zn2 O5 90.21(9) 2 .
O4 Zn2 O5 86.09(9) 2 .
O4 Zn2 O5 93.91(9) . .
O5 Zn2 O5 180.00(15) 2 .
C1 O1 Zn2 141.29(18) . .
C1 O2 Zn1 117.84(18) . .
C7 O3 Zn1 111.15(17) . .
C7 O4 Zn2 142.11(19) . .
C13 O5 Zn2 127.49(18) . .
C13 O6 Zn1 121.02(18) . .
C19 O7 Zn1 124.42(18) . .
C20 N1 C21 120.7(3) . .
C20 N1 C22 122.8(4) . .
C21 N1 C22 116.4(4) . .
O1 C1 O2 125.4(2) . .
O1 C1 C2 117.6(2) . .
O2 C1 C2 117.0(2) . .
C3 C2 C6 120.4(2) . 2_544
C3 C2 C1 118.6(2) . .
C6 C2 C1 121.0(2) 2_544 .
C2 C3 C4 121.2(3) . .
C5 C4 C3 122.4(3) . .
C5 C4 C4 119.7(3) . 2_544
C3 C4 C4 117.9(3) . 2_544
C6 C5 C4 121.0(3) . .
C5 C6 C2 119.9(3) . 2_544
O4 C7 O3 123.1(2) . .
O4 C7 C8 120.1(2) . .
O3 C7 C8 116.9(2) . .
C11 C8 C9 120.1(2) . .
C11 C8 C7 120.8(2) . .
C9 C8 C7 119.1(2) . .
C10 C9 C8 120.0(2) . .
C9 C10 C12 121.1(2) . 2_666
C8 C11 C12 121.0(2) . .
C10 C12 C11 122.2(2) 2_666 .
C10 C12 C12 119.2(3) 2_666 2_666
C11 C12 C12 118.6(3) . 2_666
O5 C13 O6 123.9(3) . .
O5 C13 C14 120.1(2) . .
O6 C13 C14 115.9(2) . .
C18 C14 C15 119.6(3) 2_445 .
C18 C14 C13 120.5(3) 2_445 .
C15 C14 C13 119.8(2) . .
C16 C15 C14 120.5(3) . .
C15 C16 C17 120.9(3) . .
C18 C17 C16 122.3(2) . .
C18 C17 C17 118.8(3) . 2_445
C16 C17 C17 118.9(3) . 2_445
C14 C18 C17 121.3(3) 2_445 .
O8 C20 N1 124.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O6 1.933(2) .
Zn1 O3 1.939(3) .
Zn1 O2 1.956(3) .
Zn1 O7 2.000(2) .
Zn2 O1 2.038(2) .
Zn2 O1 2.038(2) 2
Zn2 O4 2.110(2) 2
Zn2 O4 2.110(2) .
Zn2 O5 2.119(2) 2
Zn2 O5 2.119(2) .
O1 C1 1.248(3) .
O2 C1 1.278(3) .
O3 C7 1.286(3) .
O4 C7 1.247(3) .
O5 C13 1.259(3) .
O6 C13 1.275(3) .
O7 C19 1.429(4) .
O8 C20 1.232(4) .
O9 O9 1.366(12) 2_455
N1 C20 1.322(5) .
N1 C21 1.451(5) .
N1 C22 1.456(5) .
C1 C2 1.501(4) .
C2 C3 1.372(4) .
C2 C6 1.413(4) 2_544
C3 C4 1.419(4) .
C4 C5 1.410(4) .
C4 C4 1.428(5) 2_544
C5 C6 1.370(4) .
C6 C2 1.413(4) 2_544
C7 C8 1.501(4) .
C8 C11 1.373(4) .
C8 C9 1.424(4) .
C9 C10 1.364(4) .
C10 C12 1.418(4) 2_666
C11 C12 1.422(4) .
C12 C10 1.418(4) 2_666
C12 C12 1.422(5) 2_666
C13 C14 1.501(4) .
C14 C18 1.378(4) 2_445
C14 C15 1.422(4) .
C15 C16 1.370(4) .
C16 C17 1.424(4) .
C17 C18 1.419(4) .
C17 C17 1.426(5) 2_445
C18 C14 1.378(4) 2_445
