#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:40:03 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178789 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/43/4104330.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_4104330
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         'Co (C12 H16 O4) (H2O)'
_chemical_formula_sum            'C18 H18 Co O5'
_chemical_formula_weight         373.25
_chemical_name_common            MAMS-3
_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                   18.9328(12)
_cell_length_b                   18.9328(12)
_cell_length_c                   22.307(3)
_cell_measurement_reflns_used    3493
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.66
_cell_measurement_theta_min      2.15
_cell_volume                     6924.7(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.1489
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24266
_diffrn_reflns_theta_full        20.80
_diffrn_reflns_theta_max         20.80
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            DARK
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0665
_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)+(0.1358P)²+6.7375P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2030
_refine_ls_wR_factor_ref         0.2098
_reflns_number_gt                1928
_reflns_number_total             2427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808896f_si_003.cif
_cod_data_source_block           xamd670
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4104330
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
Co1 Co 0.95055(5) 0.46289(5) 0.19670(4) 0.0370(5) Uani 1 1 d .
O4 O 0.8922(3) 0.5103(3) 0.2456(2) 0.0514(13) Uani 1 1 d .
C15 C 0.8562(4) 0.5694(4) 0.3248(3) 0.0435(17) Uani 1 1 d .
C14 C 0.7856(4) 0.5551(4) 0.2951(3) 0.0517(19) Uani 1 1 d .
H14A H 0.7731 0.5298 0.2573 0.062 Uiso 1 1 calc R
C13 C 0.8739(4) 0.6060(4) 0.3807(3) 0.0499(18) Uani 1 1 d .
H13A H 0.9207 0.6140 0.4012 0.060 Uiso 1 1 calc R
C12 C 0.8233(4) 0.6316(4) 0.4076(3) 0.051(2) Uani 1 1 d .
C11 C 0.7536(4) 0.6160(4) 0.3765(3) 0.0536(19) Uani 1 1 d .
H11A H 0.7184 0.6319 0.3938 0.064 Uiso 1 1 calc R
C10 C 0.7337(4) 0.5782(4) 0.3214(3) 0.0470(18) Uani 1 1 d .
C9 C 0.8426(4) 0.6700(5) 0.4683(3) 0.0488(18) Uani 1 1 d .
C8 C 0.9097(4) 0.5395(4) 0.2978(3) 0.0449(18) Uani 1 1 d .
C7 C 0.8722(5) 0.6415(5) 0.5133(4) 0.072(2) Uani 1 1 d .
H7A H 0.8831 0.5992 0.5049 0.087 Uiso 1 1 calc R
C5 C 0.8694(5) 0.7345(5) 0.5856(4) 0.062(2) Uani 1 1 d .
C4 C 0.8269(5) 0.7299(6) 0.4825(4) 0.083(3) Uani 1 1 d .
H4A H 0.8059 0.7499 0.4530 0.100 Uiso 1 1 calc R
C3 C 0.8412(6) 0.7627(6) 0.5395(4) 0.091(3) Uani 1 1 d .
H3A H 0.8313 0.8058 0.5472 0.109 Uiso 1 1 calc R
C2 C 0.8859(5) 0.6741(6) 0.5702(4) 0.077(2) Uani 1 1 d .
H2A H 0.9072 0.6542 0.5994 0.092 Uiso 1 1 calc R
C1 C 0.8819(6) 0.7682(7) 0.6499(5) 0.096(3) Uani 1 1 d .
O2 O 0.6424(3) 0.5275(3) 0.2395(3) 0.0721(16) Uani 1 1 d .
C6 C 0.6544(5) 0.5563(5) 0.2915(4) 0.059(2) Uani 1 1 d .
O3 O 0.9680(3) 0.5470(3) 0.3287(2) 0.0515(13) Uani 1 1 d .
O1W O 0.8885(5) 0.4346(4) 0.1195(3) 0.109(3) Uani 1 1 d .
C18 C 0.9182(12) 0.7306(10) 0.6902(5) 0.191(7) Uani 1 1 d .
H18A H 0.9739 0.7490 0.6780 0.287 Uiso 1 1 calc R
H18B H 0.8863 0.6717 0.6872 0.287 Uiso 1 1 calc R
H18C H 0.9177 0.7470 0.7313 0.287 Uiso 1 1 calc R
C17 C 0.8002(11) 0.7321(16) 0.6800(6) 0.309(16) Uani 1 1 d .
H17A H 0.7671 0.7510 0.6600 0.464 Uiso 1 1 calc R
H17B H 0.8076 0.7490 0.7217 0.464 Uiso 1 1 calc R
H17C H 0.7730 0.6731 0.6779 0.464 Uiso 1 1 calc R
C16 C 0.9333(16) 0.8578(9) 0.6491(7) 0.42(3) Uani 1 1 d .
H16A H 0.9832 0.8730 0.6273 0.623 Uiso 1 1 calc R
H16B H 0.9464 0.8779 0.6899 0.623 Uiso 1 1 calc R
H16C H 0.9041 0.8813 0.6296 0.623 Uiso 1 1 calc R
O1 O 0.6048(3) 0.5682(3) 0.3216(2) 0.0735(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'
Co Co 0.3494 0.9721 '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
O1W Co1 O2 99.0(3) . 3_665
O1W Co1 O1 101.4(3) . 5_665
O2 Co1 O1 89.7(2) 3_665 5_665
O1W Co1 O3 94.4(2) . 6_765
O2 Co1 O3 166.6(2) 3_665 6_765
O1 Co1 O3 88.4(2) 5_665 6_765
O1W Co1 O4 101.6(2) . .
O2 Co1 O4 88.9(2) 3_665 .
O1 Co1 O4 156.8(2) 5_665 .
O3 Co1 O4 87.59(18) 6_765 .
O1W Co1 Co1 176.0(2) . 6_765
O2 Co1 Co1 84.68(19) 3_665 6_765
O1 Co1 Co1 76.98(17) 5_665 6_765
O3 Co1 Co1 81.95(13) 6_765 6_765
O4 Co1 Co1 79.86(13) . 6_765
C8 O4 Co1 127.0(4) . .
C13 C15 C14 119.6(6) . .
C13 C15 C8 120.5(6) . .
C14 C15 C8 119.8(6) . .
C15 C14 C10 120.0(7) . .
C15 C14 H14A 120.0 . .
C10 C14 H14A 120.0 . .
C15 C13 C12 121.4(6) . .
C15 C13 H13A 119.3 . .
C12 C13 H13A 119.3 . .
C11 C12 C13 117.1(7) . .
C11 C12 C9 122.1(6) . .
C13 C12 C9 120.7(6) . .
C10 C11 C12 122.7(6) . .
C10 C11 H11A 118.7 . .
C12 C11 H11A 118.7 . .
C11 C10 C14 119.2(6) . .
C11 C10 C6 121.1(7) . .
C14 C10 C6 119.6(7) . .
C4 C9 C7 117.4(7) . .
C4 C9 C12 121.4(6) . .
C7 C9 C12 121.1(6) . .
O3 C8 O4 125.7(6) . .
O3 C8 C15 117.3(6) . .
O4 C8 C15 117.0(6) . .
C9 C7 C2 121.0(8) . .
C9 C7 H7A 119.5 . .
C2 C7 H7A 119.5 . .
C2 C5 C3 115.2(8) . .
C2 C5 C1 121.9(8) . .
C3 C5 C1 122.9(8) . .
C9 C4 C3 121.3(8) . .
C9 C4 H4A 119.4 . .
C3 C4 H4A 119.4 . .
C5 C3 C4 122.6(8) . .
C5 C3 H3A 118.7 . .
C4 C3 H3A 118.7 . .
C5 C2 C7 122.4(8) . .
C5 C2 H2A 118.8 . .
C7 C2 H2A 118.8 . .
C16 C1 C17 117.8(15) . .
C16 C1 C18 110.7(14) . .
C17 C1 C18 97.3(15) . .
C16 C1 C5 110.0(11) . .
C17 C1 C5 108.7(9) . .
C18 C1 C5 111.8(8) . .
C6 O2 Co1 122.7(5) . 2_655
O2 C6 O1 125.4(7) . .
O2 C6 C10 118.1(7) . .
O1 C6 C10 116.4(8) . .
C8 O3 Co1 125.5(4) . 6_765
C1 C18 H18A 109.5 . .
C1 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C1 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C1 C17 H17A 109.5 . .
C1 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C1 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C1 C16 H16A 109.5 . .
C1 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C1 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C6 O1 Co1 130.0(6) . 5_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1W 2.000(5) .
Co1 O2 1.987(5) 3_665
Co1 O1 2.031(5) 5_665
Co1 O3 2.035(4) 6_765
Co1 O4 2.051(4) .
Co1 Co1 2.8781(16) 6_765
O4 C8 1.261(8) .
C15 C13 1.385(9) .
C15 C14 1.391(9) .
C15 C8 1.510(9) .
C14 C10 1.390(9) .
C14 H14A 0.9400 .
C13 C12 1.405(9) .
C13 H13A 0.9400 .
C12 C11 1.385(10) .
C12 C9 1.493(10) .
C11 C10 1.378(9) .
C11 H11A 0.9400 .
C10 C6 1.499(10) .
C9 C4 1.346(11) .
C9 C7 1.384(10) .
C8 O3 1.247(8) .
C7 C2 1.377(10) .
C7 H7A 0.9400 .
C5 C2 1.371(11) .
C5 C3 1.384(12) .
C5 C1 1.538(12) .
C4 C3 1.381(11) .
C4 H4A 0.9400 .
C3 H3A 0.9400 .
C2 H2A 0.9400 .
C1 C16 1.474(19) .
C1 C17 1.502(18) .
C1 C18 1.510(16) .
O2 C6 1.253(9) .
O2 Co1 1.987(5) 2_655
C6 O1 1.264(9) .
O3 Co1 2.035(4) 6_765
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C18 H18C 0.9700 .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C17 H17C 0.9700 .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C16 H16C 0.9700 .
O1 Co1 2.031(5) 5_565
