#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:40:03 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178789 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/43/4104331.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_4104331
loop_
_publ_author_name
'Shengqian Ma'
'Daofeng Sun'
'Daqiang Yuan'
'Xi-Sen Wang'
'Hong-Cai Zhou'
_publ_section_title
;
 Preparation and Gas Adsorption Studies of Three Mesh-Adjustable Molecular
 Sieves with a Common Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6445
_journal_page_last               6451
_journal_paper_doi               10.1021/ja808896f
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'Cu (C12 H16 O4) (H2O)'
_chemical_formula_sum            'C18 H18 Cu O5'
_chemical_formula_weight         377.86
_chemical_name_common            MAMS-4
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_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                120.00
_cell_formula_units_Z            12
_cell_length_a                   18.4472(4)
_cell_length_b                   18.4472(4)
_cell_length_c                   22.5760(12)
_cell_measurement_temperature    213(2)
_cell_volume                     6653.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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      213(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1469
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22294
_diffrn_reflns_theta_full        20.87
_diffrn_reflns_theta_max         20.87
_diffrn_reflns_theta_min         1.27
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            turquoise
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0731
_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)+(0.1328P)²+16.6492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2152
_refine_ls_wR_factor_ref         0.2268
_reflns_number_gt                1766
_reflns_number_total             2353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808896f_si_004.cif
_cod_data_source_block           xamd676
_cod_database_code               4104331
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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
Cu1 Cu 0.50921(6) 0.04819(6) 0.29769(4) 0.0384(5) Uani 1 1 d .
O1 O 0.4711(4) 0.1138(3) 0.2550(3) 0.0501(16) Uani 1 1 d .
C1 C 0.3832(5) 0.1393(6) 0.1190(4) 0.050(2) Uani 1 1 d .
H1 H 0.3653 0.0872 0.1019 0.060 Uiso 1 1 calc R
C13 C 0.4384(5) 0.0941(6) 0.2052(4) 0.041(2) Uani 1 1 d .
C7 C 0.3336(6) 0.1767(5) 0.0291(4) 0.050(2) Uani 1 1 d .
C6 C 0.3709(6) 0.1969(5) 0.0888(4) 0.050(2) Uani 1 1 d .
C5 C 0.3968(5) 0.2733(6) 0.1163(4) 0.055(3) Uani 1 1 d .
H5 H 0.3896 0.3138 0.0970 0.066 Uiso 1 1 calc R
C2 C 0.4223(5) 0.1565(5) 0.1757(4) 0.045(2) Uani 1 1 d .
C3 C 0.4463(5) 0.2331(5) 0.2014(4) 0.047(2) Uani 1 1 d .
H3 H 0.4712 0.2451 0.2386 0.056 Uiso 1 1 calc R
C4 C 0.4342(5) 0.2909(5) 0.1734(4) 0.045(2) Uani 1 1 d .
C8 C 0.2693(6) 0.1005(6) 0.0135(5) 0.066(3) Uani 1 1 d .
H8 H 0.2449 0.0597 0.0427 0.079 Uiso 1 1 calc R
C10 C 0.2717(6) 0.1402(6) -0.0878(4) 0.061(3) Uani 1 1 d .
C12 C 0.3641(7) 0.2364(6) -0.0162(5) 0.072(3) Uani 1 1 d .
H12 H 0.4068 0.2904 -0.0078 0.086 Uiso 1 1 calc R
C9 C 0.2385(7) 0.0804(7) -0.0426(5) 0.078(3) Uani 1 1 d .
H9 H 0.1952 0.0266 -0.0509 0.094 Uiso 1 1 calc R
C11 C 0.3320(7) 0.2169(7) -0.0738(5) 0.069(3) Uani 1 1 d .
H11 H 0.3533 0.2583 -0.1027 0.083 Uiso 1 1 calc R
C15 C 0.2406(9) 0.1179(7) -0.1521(5) 0.079(3) Uani 1 1 d .
O5 O 0.5438(6) 0.1181(8) 0.3720(5) 0.162(5) Uani 1 1 d .
C17 C 0.2586(19) 0.1844(12) -0.1878(9) 0.249(15) Uani 1 1 d .
H17A H 0.3172 0.2247 -0.1853 0.374 Uiso 1 1 calc R
H17B H 0.2267 0.2099 -0.1752 0.374 Uiso 1 1 calc R
H17C H 0.2444 0.1656 -0.2280 0.374 Uiso 1 1 calc R
C18 C 0.1604(12) 0.058(2) -0.1540(11) 0.42(3) Uani 1 1 d .
H18A H 0.1266 0.0776 -0.1355 0.634 Uiso 1 1 calc R
H18B H 0.1534 0.0093 -0.1335 0.634 Uiso 1 1 calc R
H18C H 0.1434 0.0438 -0.1946 0.634 Uiso 1 1 calc R
C19 C 0.282(2) 0.086(2) -0.1798(10) 0.32(2) Uani 1 1 d .
H19A H 0.3407 0.1256 -0.1796 0.480 Uiso 1 1 calc R
H19B H 0.2624 0.0726 -0.2200 0.480 Uiso 1 1 calc R
H19C H 0.2720 0.0356 -0.1599 0.480 Uiso 1 1 calc R
C16 C 0.4623(6) 0.3753(7) 0.2012(5) 0.062(3) Uani 1 1 d .
O2 O 0.4560(4) 0.4299(4) 0.1704(3) 0.0530(16) Uani 1 1 d .
O4 O 0.4936(4) 0.3853(4) 0.2524(3) 0.0554(17) Uani 1 1 d .
O3 O 0.4237(4) 0.0301(3) 0.1760(3) 0.0494(16) 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'
O O 0.0106 0.0060 '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'
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 Cu1 O1 171.7(3) 6_655 .
O2 Cu1 O4 90.4(3) 6_655 2_655
O1 Cu1 O4 87.5(3) . 2_655
O2 Cu1 O3 89.4(3) 6_655 5
O1 Cu1 O3 90.5(2) . 5
O4 Cu1 O3 164.9(3) 2_655 5
O2 Cu1 O5 91.9(4) 6_655 .
O1 Cu1 O5 96.4(4) . .
O4 Cu1 O5 99.5(4) 2_655 .
O3 Cu1 O5 95.6(4) 5 .
O2 Cu1 Cu1 86.90(19) 6_655 5
O1 Cu1 Cu1 84.83(18) . 5
O4 Cu1 Cu1 82.01(19) 2_655 5
O3 Cu1 Cu1 82.89(17) 5 5
O5 Cu1 Cu1 178.1(4) . 5
C13 O1 Cu1 123.0(5) . .
C6 C1 C2 122.4(8) . .
C6 C1 H1 118.8 . .
C2 C1 H1 118.8 . .
O1 C13 O3 126.5(8) . .
O1 C13 C2 115.9(8) . .
O3 C13 C2 117.3(8) . .
C8 C7 C12 115.2(9) . .
C8 C7 C6 123.7(8) . .
C12 C7 C6 121.1(9) . .
C1 C6 C5 117.1(8) . .
C1 C6 C7 119.7(8) . .
C5 C6 C7 123.1(8) . .
C6 C5 C4 121.4(8) . .
C6 C5 H5 119.3 . .
C4 C5 H5 119.3 . .
C3 C2 C1 118.2(8) . .
C3 C2 C13 121.3(8) . .
C1 C2 C13 120.5(8) . .
C4 C3 C2 121.1(8) . .
C4 C3 H3 119.4 . .
C2 C3 H3 119.4 . .
C3 C4 C5 119.8(8) . .
C3 C4 C16 120.9(9) . .
C5 C4 C16 119.4(9) . .
C7 C8 C9 123.6(9) . .
C7 C8 H8 118.2 . .
C9 C8 H8 118.2 . .
C11 C10 C9 117.9(10) . .
C11 C10 C15 120.7(10) . .
C9 C10 C15 121.3(10) . .
C7 C12 C11 121.7(9) . .
C7 C12 H12 119.2 . .
C11 C12 H12 119.2 . .
C8 C9 C10 120.4(10) . .
C8 C9 H9 119.8 . .
C10 C9 H9 119.8 . .
C10 C11 C12 121.1(10) . .
C10 C11 H11 119.5 . .
C12 C11 H11 119.5 . .
C19 C15 C18 105(2) . .
C19 C15 C17 101(2) . .
C18 C15 C17 113(2) . .
C19 C15 C10 110.1(14) . .
C18 C15 C10 111.4(15) . .
C17 C15 C10 115.3(12) . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C15 C18 H18A 109.5 . .
C15 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C15 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C15 C19 H19A 109.5 . .
C15 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C15 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
O4 C16 O2 126.8(9) . .
O4 C16 C4 115.3(10) . .
O2 C16 C4 117.8(9) . .
C16 O2 Cu1 120.5(6) . 6_665
C16 O4 Cu1 123.8(7) . 3_665
C13 O3 Cu1 122.5(5) . 5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.921(6) 6_655
Cu1 O1 1.934(6) .
Cu1 O4 1.976(6) 2_655
Cu1 O3 1.977(5) 5
Cu1 O5 2.016(9) .
Cu1 Cu1 2.6472(19) 5
O1 C13 1.241(10) .
C1 C6 1.375(12) .
C1 C2 1.424(12) .
C1 H1 0.9300 .
C13 O3 1.258(10) .
C13 C2 1.482(12) .
C7 C8 1.357(13) .
C7 C12 1.397(13) .
C7 C6 1.474(13) .
C6 C5 1.389(12) .
C5 C4 1.421(12) .
C5 H5 0.9300 .
C2 C3 1.380(11) .
C3 C4 1.351(11) .
C3 H3 0.9300 .
C4 C16 1.509(13) .
C8 C9 1.360(13) .
C8 H8 0.9300 .
C10 C11 1.329(13) .
C10 C9 1.401(14) .
C10 C15 1.537(15) .
C12 C11 1.399(14) .
C12 H12 0.9300 .
C9 H9 0.9300 .
C11 H11 0.9300 .
C15 C19 1.33(3) .
C15 C18 1.33(2) .
C15 C17 1.364(19) .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C16 O4 1.262(11) .
C16 O2 1.276(12) .
O2 Cu1 1.921(6) 6_665
O4 Cu1 1.976(6) 3_665
O3 Cu1 1.977(5) 5
