#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:58:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179402 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/99/4329956.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_4329956
loop_
_publ_author_name
'Elena Ilyes'
'Mihaela Florea'
'Augustin M. Madalan'
'Ionel Haiduc'
'Vasile I. Parvulescu'
'Marius Andruh'
_publ_section_title
;
 A Robust Metal-Organic Framework Constructed from Alkoxo-Bridged
 Binuclear Nodes and Hexamethylenetetramine Spacers: Crystal Structure and
 Sorption Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7954
_journal_page_last               7956
_journal_paper_doi               10.1021/ic301139j
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C22 H26 Cu2 N4 O7'
_chemical_formula_weight         585.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                   17.5087(11)
_cell_length_b                   17.5087(11)
_cell_length_c                   15.1964(12)
_cell_measurement_reflns_used    12812
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.93
_cell_volume                     4658.5(6)
_computing_cell_refinement       X-Area
_computing_data_collection       X-Area
_computing_data_reduction        X-Area
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       '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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16449
_diffrn_reflns_theta_full        28.41
_diffrn_reflns_theta_max         28.41
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    1.878
_exptl_absorpt_correction_T_max  0.7258
_exptl_absorpt_correction_T_min  0.6607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       prism
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0358P)²+3.5849P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                2359
_reflns_number_total             2895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301139j_si_001.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4329956
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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 0.59743(15) 0.90224(15) 0.14556(17) 0.0257(5) Uani 1 1 d .
C2 C 0.57610(18) 0.98804(15) 0.14551(17) 0.0311(6) Uani 1 1 d .
H2 H 0.6226 1.0185 0.1375 0.037 Uiso 1 1 calc R
C3 C 0.5404(2) 1.00770(16) 0.23418(19) 0.0417(8) Uani 1 1 d .
C4 C 0.5843(3) 1.0349(2) 0.3035(2) 0.0694(13) Uani 1 1 d .
H4 H 0.6367 1.0404 0.2961 0.083 Uiso 1 1 calc R
C5 C 0.5516(5) 1.0538(3) 0.3829(3) 0.0914(19) Uani 1 1 d .
H5 H 0.5817 1.0721 0.4287 0.110 Uiso 1 1 calc R
C6 C 0.4755(5) 1.0455(3) 0.3940(3) 0.096(2) Uani 1 1 d .
H6 H 0.4534 1.0591 0.4474 0.115 Uiso 1 1 calc R
C7 C 0.4308(4) 1.0176(3) 0.3285(3) 0.0820(16) Uani 1 1 d .
H7 H 0.3787 1.0112 0.3377 0.098 Uiso 1 1 calc R
C8 C 0.4630(3) 0.99849(19) 0.2469(2) 0.0553(10) Uani 1 1 d .
H8 H 0.4324 0.9797 0.2018 0.066 Uiso 1 1 calc R
C9 C 0.5000 0.7500 -0.0188(2) 0.0225(7) Uani 1 2 d S
H9A H 0.5447 0.7526 0.0188 0.027 Uiso 0.50 1 calc PR
H9B H 0.4553 0.7474 0.0188 0.027 Uiso 0.50 1 calc PR
C10 C 0.42712(16) 0.81346(15) -0.13114(18) 0.0275(6) Uani 1 1 d .
H10A H 0.3817 0.8110 -0.0947 0.033 Uiso 1 1 calc R
H10B H 0.4232 0.8585 -0.1681 0.033 Uiso 1 1 calc R
C11 C 0.56481(16) 0.82182(15) -0.13121(19) 0.0294(6) Uani 1 1 d .
H11A H 0.5632 0.8670 -0.1682 0.035 Uiso 1 1 calc R
H11B H 0.6103 0.8249 -0.0949 0.035 Uiso 1 1 calc R
C12 C 0.5000 0.7500 -0.2407(2) 0.0357(9) Uani 1 2 d S
H12A H 0.5027 0.7053 -0.2782 0.043 Uiso 0.50 1 calc PR
H12B H 0.4973 0.7947 -0.2782 0.043 Uiso 0.50 1 calc PR
Cu1 Cu 0.497684(19) 0.914516(16) 0.006832(19) 0.02187(10) Uani 1 1 d .
N1 N 0.49583(12) 0.82038(11) -0.07352(13) 0.0196(4) Uani 1 1 d .
N2 N 0.56923(14) 0.75417(13) -0.18654(15) 0.0319(5) Uani 1 1 d .
O1 O 0.56571(12) 0.86166(11) 0.08817(13) 0.0342(5) Uani 1 1 d .
O2 O 0.64243(12) 0.87760(11) 0.20197(13) 0.0367(5) Uani 1 1 d .
O3 O 0.52598(11) 1.00289(10) 0.07601(11) 0.0266(4) Uani 1 1 d .
O4W O 0.2731(12) 0.9638(16) 0.265(2) 0.41(2) Uani 0.50 1 d P
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'
Cu Cu 0.3201 1.2651 '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'
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
O2 C1 O1 124.3(2) . .
O2 C1 C2 119.4(2) . .
O1 C1 C2 116.3(2) . .
O3 C2 C3 111.6(3) . .
O3 C2 C1 109.4(2) . .
C3 C2 C1 108.5(2) . .
O3 C2 H2 109.1 . .
C3 C2 H2 109.1 . .
C1 C2 H2 109.1 . .
C8 C3 C4 118.5(4) . .
C8 C3 C2 120.0(3) . .
C4 C3 C2 121.4(4) . .
C5 C4 C3 121.2(5) . .
C5 C4 H4 119.4 . .
C3 C4 H4 119.4 . .
C6 C5 C4 119.6(5) . .
C6 C5 H5 120.2 . .
C4 C5 H5 120.2 . .
C5 C6 C7 121.1(5) . .
C5 C6 H6 119.5 . .
C7 C6 H6 119.5 . .
C6 C7 C8 120.1(6) . .
C6 C7 H7 119.9 . .
C8 C7 H7 119.9 . .
C3 C8 C7 119.4(4) . .
C3 C8 H8 120.3 . .
C7 C8 H8 120.3 . .
N1 C9 N1 112.1(3) 6_564 .
N1 C9 H9A 109.2 6_564 .
N1 C9 H9A 109.2 . .
N1 C9 H9B 109.2 6_564 .
N1 C9 H9B 109.2 . .
H9A C9 H9B 107.9 . .
N2 C10 N1 111.7(2) 6_564 .
N2 C10 H10A 109.3 6_564 .
N1 C10 H10A 109.3 . .
N2 C10 H10B 109.3 6_564 .
N1 C10 H10B 109.3 . .
H10A C10 H10B 107.9 . .
N2 C11 N1 111.6(2) . .
N2 C11 H11A 109.3 . .
N1 C11 H11A 109.3 . .
N2 C11 H11B 109.3 . .
N1 C11 H11B 109.3 . .
H11A C11 H11B 108.0 . .
N2 C12 N2 111.8(3) . 6_564
N2 C12 H12A 109.3 . .
N2 C12 H12A 109.3 6_564 .
N2 C12 H12B 109.3 . .
N2 C12 H12B 109.3 6_564 .
H12A C12 H12B 107.9 . .
O3 Cu1 O1 83.04(7) . .
O3 Cu1 O3 79.23(8) . 9_675
O1 Cu1 O3 152.33(9) . 9_675
O3 Cu1 N1 165.88(9) . .
O1 Cu1 N1 90.32(8) . .
O3 Cu1 N1 101.95(7) 9_675 .
O3 Cu1 O2 103.26(8) . 12_766
O1 Cu1 O2 109.16(8) . 12_766
O3 Cu1 O2 95.54(8) 9_675 12_766
N1 Cu1 O2 90.68(8) . 12_766
O3 Cu1 Cu1 39.94(5) . 9_675
O1 Cu1 Cu1 120.04(6) . 9_675
O3 Cu1 Cu1 39.30(5) 9_675 9_675
N1 Cu1 Cu1 139.51(6) . 9_675
O2 Cu1 Cu1 102.18(6) 12_766 9_675
C9 N1 C11 107.60(17) . .
C9 N1 C10 107.45(17) . .
C11 N1 C10 108.0(2) . .
C9 N1 Cu1 109.39(15) . .
C11 N1 Cu1 108.86(15) . .
C10 N1 Cu1 115.28(15) . .
C10 N2 C11 109.3(2) 6_564 .
C10 N2 C12 108.7(2) 6_564 .
C11 N2 C12 108.7(2) . .
C1 O1 Cu1 116.26(17) . .
C1 O2 Cu1 128.48(18) . 15_565
C2 O3 Cu1 115.00(15) . .
C2 O3 Cu1 139.01(16) . 9_675
Cu1 O3 Cu1 100.77(8) . 9_675
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.242(3) .
C1 O1 1.255(3) .
C1 C2 1.548(4) .
C2 O3 1.398(3) .
C2 C3 1.525(4) .
C2 H2 0.9800 .
C3 C8 1.378(6) .
C3 C4 1.387(5) .
C4 C5 1.376(7) .
C4 H4 0.9300 .
C5 C6 1.350(9) .
C5 H5 0.9300 .
C6 C7 1.357(8) .
C6 H6 0.9300 .
C7 C8 1.403(5) .
C7 H7 0.9300 .
C8 H8 0.9300 .
C9 N1 1.488(3) 6_564
C9 N1 1.488(3) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 N2 1.454(3) 6_564
C10 N1 1.493(3) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 N2 1.455(4) .
C11 N1 1.493(3) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 N2 1.467(3) .
C12 N2 1.467(3) 6_564
C12 H12A 0.9700 .
C12 H12B 0.9700 .
Cu1 O3 1.9351(17) .
Cu1 O1 1.9500(19) .
Cu1 O3 1.9616(17) 9_675
Cu1 N1 2.0514(19) .
Cu1 O2 2.314(2) 12_766
Cu1 Cu1 3.0017(6) 9_675
N2 C10 1.454(3) 6_564
O2 Cu1 2.314(2) 15_565
O3 Cu1 1.9616(17) 9_675
