#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:18:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179054 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/16/4301651.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_4301651
loop_
_publ_author_name
'Shuting Wu'
'Liqing Ma'
'La-Sheng Long'
'Lan-Sun Zheng'
'Wenbin Lin'
_publ_section_title
;
Three-Dimensional Metal-Organic Frameworks Based on Functionalized
Tetracarboxylate Linkers: Synthesis, Strucures, and Gas Sorption Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2436
_journal_page_last               2442
_journal_paper_doi               10.1021/ic801631w
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C20 H11 Cu N0 O7'
_chemical_formula_weight         426.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           66
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2 2c'
_symmetry_space_group_name_H-M   'C c c m'
_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            8
_cell_length_a                   15.9568(15)
_cell_length_b                   29.329(2)
_cell_length_c                   28.657(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.845
_cell_measurement_theta_min      0.793
_cell_volume                     13411.4(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17727
_diffrn_reflns_theta_full        49.98
_diffrn_reflns_theta_max         49.98
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.8498
_exptl_absorpt_correction_T_min  0.7668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    0.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.030
_refine_ls_extinction_coef       0.000023(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         3486
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0571
_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)+(0.1072P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1708
_reflns_number_gt                1997
_reflns_number_total             3486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801631w_si_001_1.cif
_cod_data_source_block           5
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        13411.3(19)
_cod_database_code               4301651
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z-1/2'
'-x, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, 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_assembly
_atom_site_disorder_group
Cu1 Cu 0.18503(5) 0.22270(2) 0.0000 0.1145(5) Uani 1 2 d SU . .
C1 C 0.1851(4) 0.29853(16) -0.06211(15) 0.1176(14) Uani 1 1 d U . .
O1 O 0.2543(2) 0.31019(9) -0.04801(9) 0.1261(11) Uani 1 1 d U . .
O2 O 0.1420(2) 0.26355(9) -0.04804(9) 0.1343(11) Uani 1 1 d U . .
C9 C 0.0340(3) 0.45006(14) -0.21432(15) 0.1276(15) Uani 1 1 d U . .
C8 C 0.0364(3) 0.40236(12) -0.21307(14) 0.1259(15) Uani 1 1 d U . .
C3 C 0.1854(3) 0.36386(16) -0.11829(16) 0.1388(16) Uani 1 1 d U . .
H3A H 0.2360 0.3733 -0.1054 0.167 Uiso 1 1 calc R . .
C2 C 0.1463(4) 0.32489(15) -0.10120(17) 0.1281(14) Uani 1 1 d U . .
C7 C 0.0701(4) 0.31303(15) -0.11967(17) 0.1423(16) Uani 1 1 d U . .
H7A H 0.0422 0.2877 -0.1078 0.171 Uiso 1 1 calc R . .
C10 C 0.0000 0.47427(16) -0.2500 0.1187(18) Uani 1 2 d SU . .
O1W O 0.0776(3) 0.17895(14) 0.0000 0.1815(18) Uani 1 2 d SU . .
C4 C 0.1493(4) 0.38909(15) -0.15466(18) 0.1495(17) Uani 1 1 d U . .
H4A H 0.1774 0.4145 -0.1663 0.179 Uiso 1 1 calc R . .
C5 C 0.0728(4) 0.37699(14) -0.17363(16) 0.1246(14) Uani 1 1 d U . .
C6 C 0.0327(3) 0.33813(15) -0.15620(16) 0.1439(16) Uani 1 1 d U . .
H6A H -0.0183 0.3289 -0.1686 0.173 Uiso 1 1 calc R . .
C11 C 0.0000 0.38008(18) -0.2500 0.1299(19) Uani 1 2 d SU . .
H11A H 0.0000 0.3484 -0.2500 0.156 Uiso 1 2 calc SR . .
O3 O 0.0724(3) 0.47183(15) -0.17709(19) 0.276(2) Uani 1 1 d U . .
H1W H -0.001(8) 0.179(6) 0.017(10) 0.96(13) Uiso 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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
_geom_angle_publ_flag
O1 Cu1 O1 90.38(17) 6 13 ?
O1 Cu1 O2 169.21(12) 6 10 ?
O1 Cu1 O2 88.89(11) 13 10 ?
O1 Cu1 O2 88.89(11) 6 . ?
O1 Cu1 O2 169.21(12) 13 . ?
O2 Cu1 O2 89.82(16) 10 . ?
O1 Cu1 O1W 95.84(13) 6 . ?
O1 Cu1 O1W 95.84(13) 13 . ?
O2 Cu1 O1W 94.94(13) 10 . ?
O2 Cu1 O1W 94.94(13) . . ?
O1 Cu1 Cu1 84.77(10) 6 13 ?
O1 Cu1 Cu1 84.77(10) 13 13 ?
O2 Cu1 Cu1 84.44(9) 10 13 ?
O2 Cu1 Cu1 84.44(9) . 13 ?
O1W Cu1 Cu1 179.12(14) . 13 ?
O1 C1 O2 126.5(4) . . ?
O1 C1 C2 118.4(5) . . ?
O2 C1 C2 114.9(5) . . ?
C1 O1 Cu1 123.1(3) . 13 ?
C1 O2 Cu1 121.2(3) . . ?
C10 C9 O3 121.0(4) . . ?
C10 C9 C8 123.6(4) . . ?
O3 C9 C8 115.4(4) . . ?
C11 C8 C9 116.4(4) . . ?
C11 C8 C5 121.2(4) . . ?
C9 C8 C5 122.4(4) . . ?
C2 C3 C4 120.8(5) . . ?
C7 C2 C3 118.0(5) . . ?
C7 C2 C1 121.7(5) . . ?
C3 C2 C1 120.2(6) . . ?
C2 C7 C6 121.9(5) . . ?
C9 C10 C9 116.9(5) 3_554 . ?
C9 C10 C10 121.5(2) 3_554 2_565 ?
C9 C10 C10 121.5(2) . 2_565 ?
C5 C4 C3 121.3(5) . . ?
C4 C5 C6 118.2(5) . . ?
C4 C5 C8 121.3(4) . . ?
C6 C5 C8 120.4(5) . . ?
C5 C6 C7 119.8(5) . . ?
C8 C11 C8 123.2(5) . 3_554 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.939(3) 6 ?
Cu1 O1 1.939(3) 13 ?
Cu1 O2 1.950(3) 10 ?
Cu1 O2 1.950(3) . ?
Cu1 O1W 2.142(5) . ?
Cu1 Cu1 2.6196(15) 13 ?
C1 O1 1.224(5) . ?
C1 O2 1.299(5) . ?
C1 C2 1.495(6) . ?
O1 Cu1 1.939(3) 13 ?
C9 C10 1.358(4) . ?
C9 O3 1.386(5) . ?
C9 C8 1.400(5) . ?
C8 C11 1.373(4) . ?
C8 C5 1.472(5) . ?
C3 C2 1.391(5) . ?
C3 C4 1.402(5) . ?
C2 C7 1.372(5) . ?
C7 C6 1.412(5) . ?
C10 C9 1.358(4) 3_554 ?
C10 C10 1.509(10) 2_565 ?
C4 C5 1.383(5) . ?
C5 C6 1.399(5) . ?
C11 C8 1.373(4) 3_554 ?
