#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:43:07 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178960 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/89/4118954.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_4118954
loop_
_publ_author_name
'Mona H. Mohamed'
'Sameh K. Elsaidi'
'Lukasz Wojtas'
'Tony Pham'
'Katherine A. Forrest'
'Brant Tudor'
'Brian Space'
'Michael J. Zaworotko'
_publ_section_title
;
 Highly Selective CO2 Uptake in Uninodal 6-Connected "mmo" Nets Based upon
 MO42- (M = Cr, Mo) Pillars
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19556
_journal_page_last               19559
_journal_paper_doi               10.1021/ja309452y
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C25.33 H20 Co Mo N4.67 O9.36'
_chemical_formula_weight         694.39
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_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            9
_cell_length_a                   21.3191(3)
_cell_length_b                   21.3191(3)
_cell_length_c                   17.9250(3)
_cell_measurement_temperature    228(2)
_cell_volume                     7055.50(18)
_computing_cell_refinement       'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)'
_computing_publication_material  'APEX2 (Bruker, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008); OLEX2 (2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      228(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'omega scans'
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14736
_diffrn_reflns_theta_full        68.35
_diffrn_reflns_theta_max         68.35
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    7.901
_exptl_absorpt_correction_T_max  0.4769
_exptl_absorpt_correction_T_min  0.4042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       block
_exptl_crystal_F_000             3137
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         2787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0241
_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)+(0.0361P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0577
_reflns_number_gt                2704
_reflns_number_total             2787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja309452y_si_004.cif
_cod_data_source_block           MOOFOUR-1-Co
_cod_original_cell_volume        7055.49(18)
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               4118954
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'
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 0.31171(17) 0.10758(17) 0.80976(17) 0.0260(7) Uani 1 1 d .
H1 H 0.2739 0.0928 0.8445 0.031 Uiso 1 1 calc R
C2 C 0.34584(19) 0.17830(19) 0.78540(18) 0.0320(7) Uani 1 1 d .
H2 H 0.3312 0.2105 0.8032 0.038 Uiso 1 1 calc R
C3 C 0.40209(18) 0.20175(17) 0.73422(17) 0.0304(7) Uani 1 1 d .
C4 C 0.42201(18) 0.15174(18) 0.71190(18) 0.0300(7) Uani 1 1 d .
H4 H 0.4609 0.1657 0.6787 0.036 Uiso 1 1 calc R
C5 C 0.38497(15) 0.08207(18) 0.73826(14) 0.0228(6) Uani 1 1 d .
H5 H 0.3989 0.0490 0.7218 0.027 Uiso 1 1 calc R
C6 C 0.4360(2) 0.27595(18) 0.7054(2) 0.0389(9) Uani 1 1 d .
H6 H 0.4187 0.3057 0.7238 0.047 Uiso 1 1 calc R
C7 C 0.4890(2) 0.3047(2) 0.6557(2) 0.0452(10) Uani 1 1 d .
H7 H 0.5088 0.2762 0.6400 0.054 Uiso 1 1 calc R
C8 C 0.5195(2) 0.37752(19) 0.6230(2) 0.0388(9) Uani 1 1 d .
C9 C 0.5814(2) 0.4047(2) 0.5786(2) 0.0454(10) Uani 1 1 d .
H9 H 0.6050 0.3778 0.5715 0.054 Uiso 1 1 calc R
C10 C 0.60746(19) 0.47159(18) 0.5454(2) 0.0325(8) Uani 1 1 d .
H10 H 0.6492 0.4893 0.5156 0.039 Uiso 1 1 calc R
C11 C 0.51813(19) 0.48615(18) 0.59667(18) 0.0310(8) Uani 1 1 d .
H11 H 0.4957 0.5141 0.6033 0.037 Uiso 1 1 calc R
C12 C 0.4887(2) 0.4203(2) 0.6322(2) 0.0398(9) Uani 1 1 d .
H12 H 0.4477 0.4046 0.6627 0.048 Uiso 1 1 calc R
Co1 Co 0.28375(3) -0.04959(3) 0.8333 0.01110(14) Uani 1 2 d S
Mo1 Mo 0.207209(13) 0.0000 1.0000 0.01520(9) Uani 1 2 d S
N1 N 0.57689(14) 0.51261(13) 0.55326(13) 0.0209(6) Uani 1 1 d .
N2 N 0.32949(12) 0.05897(13) 0.78672(11) 0.0194(5) Uani 1 1 d .
O1 O 0.19724(14) 0.07499(14) 0.98144(14) 0.0408(6) Uani 1 1 d .
O2 O 0.24703(12) -0.01694(12) 0.92172(10) 0.0225(5) Uani 1 1 d .
N21 N 0.6667 0.3333 0.7077(8) 0.158(5) Uani 1 3 d S
C21 C 0.6412(19) 0.3654(18) 0.7518(12) 0.142(10) Uani 0.33 1 d P
C22 C 0.7850(15) 0.3918(18) 0.8073(14) 0.187(14) Uani 0.33 1 d P
O3 O 0.5318(5) 0.2901(4) 0.4719(4) 0.070(3) Uani 0.395(9) 1 d P
O4 O 0.2123(4) 0.2095(4) 1.0325(5) 0.086(4) Uani 0.510(11) 1 d P
O5 O 0.3465(4) 0.3532(4) 0.7897(5) 0.109(4) Uani 0.594(12) 1 d P
O6 O 0.6826(6) 0.3827(6) 0.4385(5) 0.080(4) Uani 0.379(10) 1 d P
O7 O 0.2426(6) 0.2407(6) 0.8769(6) 0.145(6) Uani 0.632(18) 1 d P
O8 O 0.7271(6) 0.3938(6) 0.3333 0.071(6) Uani 0.339(12) 2 d SP
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'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 '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
N2 C1 C2 123.5(3) . .
N2 C1 H1 118.2 . .
C2 C1 H1 118.2 . .
C1 C2 C3 119.5(3) . .
C1 C2 H2 120.3 . .
C3 C2 H2 120.3 . .
C4 C3 C2 117.0(3) . .
C4 C3 C6 123.5(3) . .
C2 C3 C6 119.5(3) . .
C5 C4 C3 120.0(3) . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
N2 C5 C4 122.9(3) . .
N2 C5 H5 118.5 . .
C4 C5 H5 118.5 . .
C7 C6 C3 125.7(4) . .
C7 C6 H6 117.2 . .
C3 C6 H6 117.2 . .
C6 C7 C8 125.5(4) . .
C6 C7 H7 117.2 . .
C8 C7 H7 117.2 . .
C12 C8 C9 117.4(3) . .
C12 C8 C7 123.1(3) . .
C9 C8 C7 119.5(3) . .
C10 C9 C8 118.9(3) . .
C10 C9 H9 120.6 . .
C8 C9 H9 120.6 . .
N1 C10 C9 123.8(3) . .
N1 C10 H10 118.1 . .
C9 C10 H10 118.1 . .
N1 C11 C12 123.6(3) . .
N1 C11 H11 118.2 . .
C12 C11 H11 118.2 . .
C11 C12 C8 119.8(3) . .
C11 C12 H12 120.1 . .
C8 C12 H12 120.1 . .
O2 Co1 O2 177.56(13) . 18_546
O2 Co1 N1 89.23(9) . 7_445
O2 Co1 N1 89.04(9) 18_546 7_445
O2 Co1 N1 89.03(9) . 12_446
O2 Co1 N1 89.23(9) 18_546 12_446
N1 Co1 N1 89.29(14) 7_445 12_446
O2 Co1 N2 88.84(9) . .
O2 Co1 N2 93.01(9) 18_546 .
N1 Co1 N2 175.80(9) 7_445 .
N1 Co1 N2 94.40(9) 12_446 .
O2 Co1 N2 93.01(9) . 18_546
O2 Co1 N2 88.83(9) 18_546 18_546
N1 Co1 N2 94.40(9) 7_445 18_546
N1 Co1 N2 175.80(9) 12_446 18_546
N2 Co1 N2 81.98(12) . 18_546
O1 Mo1 O1 109.21(17) . 4_557
O1 Mo1 O2 110.38(12) . 4_557
O1 Mo1 O2 109.05(11) 4_557 4_557
O1 Mo1 O2 109.05(11) . .
O1 Mo1 O2 110.38(12) 4_557 .
O2 Mo1 O2 108.79(13) 4_557 .
C10 N1 C11 116.5(3) . .
C10 N1 Co1 123.7(2) . 13_554
C11 N1 Co1 119.7(2) . 13_554
C1 N2 C5 117.0(3) . .
C1 N2 Co1 123.78(18) . .
C5 N2 Co1 118.7(2) . .
Mo1 O2 Co1 172.94(14) . .
C21 N21 C21 88.1(19) 3_665 2_655
C21 N21 C21 88.1(19) 3_665 .
C21 N21 C21 88.1(19) 2_655 .
N21 C21 C22 173(3) . 2_655
N21 C21 C21 46.0(10) . 2_655
C22 C21 C21 127(3) 2_655 2_655
N21 C21 C21 46.0(10) . 3_665
C22 C21 C21 133(2) 2_655 3_665
C21 C21 C21 60.000(6) 2_655 3_665
O4 O4 O7 156.7(6) 6_557 6_557
O7 O5 O5 109.8(7) 16_556 16_556
O6 O6 O6 60.000(1) 2_655 3_665
O5 O7 O4 112.1(8) 16_556 6_557
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.335(4) .
C1 C2 1.377(4) .
C1 H1 0.9400 .
C2 C3 1.389(4) .
C2 H2 0.9400 .
C3 C4 1.389(5) .
C3 C6 1.466(4) .
C4 C5 1.371(4) .
C4 H4 0.9400 .
C5 N2 1.347(3) .
C5 H5 0.9400 .
C6 C7 1.324(5) .
C6 H6 0.9400 .
C7 C8 1.473(5) .
C7 H7 0.9400 .
C8 C12 1.374(5) .
C8 C9 1.394(5) .
C9 C10 1.381(4) .
C9 H9 0.9400 .
C10 N1 1.334(4) .
C10 H10 0.9400 .
C11 N1 1.336(4) .
C11 C12 1.374(5) .
C11 H11 0.9400 .
C12 H12 0.9400 .
Co1 O2 2.0377(18) .
Co1 O2 2.0378(18) 18_546
Co1 N1 2.167(2) 7_445
Co1 N1 2.167(2) 12_446
Co1 N2 2.179(2) .
Co1 N2 2.179(2) 18_546
Mo1 O1 1.747(2) .
Mo1 O1 1.747(2) 4_557
Mo1 O2 1.7682(18) 4_557
Mo1 O2 1.7682(18) .
N1 Co1 2.167(2) 13_554
N21 C21 1.33(3) 3_665
N21 C21 1.33(3) 2_655
N21 C21 1.33(3) .
C21 C22 1.50(3) 2_655
C21 C21 1.84(5) 2_655
C21 C21 1.84(5) 3_665
C22 C21 1.50(3) 3_665
O4 O4 1.170(18) 6_557
O4 O7 1.752(12) 6_557
O5 O7 1.685(13) 16_556
O5 O5 1.728(18) 16_556
O6 O6 1.611(17) 2_655
O6 O6 1.611(17) 3_665
O7 O5 1.685(13) 16_556
O7 O4 1.752(12) 6_557
