#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:43:07 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178960 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/89/4118955.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_4118955
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            'C26 H20 Mo N5 Ni O7.58'
_chemical_formula_weight         678.45
_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                   21.0856(9)
_cell_length_b                   21.0856(9)
_cell_length_c                   17.9678(8)
_cell_measurement_temperature    100(2)
_cell_volume                     6918.3(5)
_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)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14529
_diffrn_reflns_theta_full        17.29
_diffrn_reflns_theta_max         17.29
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.9861
_exptl_absorpt_correction_T_min  0.9724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             3075
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         4649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0322
_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)+(0.0546P)²+8.0714P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0870
_reflns_number_gt                4628
_reflns_number_total             4649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja309452y_si_005.cif
_cod_data_source_block           MOOFOUR-1-Ni
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               4118955
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 -0.14323(13) 0.05364(13) 0.21103(15) 0.0251(4) Uani 1 1 d .
H1 H -0.1612 0.0109 0.1811 0.030 Uiso 1 1 calc R
C2 C -0.07614(15) 0.07986(16) 0.24489(18) 0.0348(6) Uani 1 1 d .
H2 H -0.0489 0.0556 0.2376 0.042 Uiso 1 1 calc R
C3 C -0.04817(16) 0.14218(16) 0.28997(18) 0.0330(6) Uani 1 1 d .
C4 C -0.09130(15) 0.17520(17) 0.29721(19) 0.0364(6) Uani 1 1 d .
H4 H -0.0747 0.2181 0.3266 0.044 Uiso 1 1 calc R
C5 C -0.15789(14) 0.14504(14) 0.26150(14) 0.0268(5) Uani 1 1 d .
H5 H -0.1866 0.1678 0.2680 0.032 Uiso 1 1 calc R
C6 C -0.49383(17) -0.30846(16) 0.3439(2) 0.0392(7) Uani 1 1 d .
H6 H -0.5156 -0.2801 0.3573 0.047 Uiso 1 1 calc R
C7 C -0.43775(15) -0.27898(13) 0.29682(17) 0.0304(5) Uani 1 1 d .
H7 H -0.4181 -0.3086 0.2810 0.036 Uiso 1 1 calc R
C8 C -0.40389(12) -0.20424(12) 0.26739(13) 0.0246(4) Uani 1 1 d .
C9 C -0.34776(13) -0.18102(12) 0.21474(15) 0.0257(4) Uani 1 1 d .
H9 H -0.3331 -0.2141 0.1966 0.031 Uiso 1 1 calc R
C10 C -0.31384(12) -0.10984(12) 0.18934(13) 0.0217(4) Uani 1 1 d .
H10 H -0.2759 -0.0951 0.1534 0.026 Uiso 1 1 calc R
C11 C -0.38629(11) -0.08238(12) 0.26325(12) 0.0195(4) Uani 1 1 d .
H11 H -0.3996 -0.0480 0.2805 0.023 Uiso 1 1 calc R
C12 C -0.42356(13) -0.15310(13) 0.29064(13) 0.0239(4) Uani 1 1 d .
H12 H -0.4624 -0.1669 0.3252 0.029 Uiso 1 1 calc R
Mo1 Mo -0.208332(9) 0.0000 0.0000 0.01591(7) Uani 1 2 d S
N1 N -0.33165(9) -0.06024(10) 0.21278(9) 0.0173(3) Uani 1 1 d .
N2 N -0.18456(10) 0.08539(11) 0.21815(11) 0.0197(3) Uani 1 1 d .
Ni1 Ni -0.287371(16) 0.045962(16) 0.1667 0.01280(8) Uani 1 2 d S
O1 O -0.12227(10) 0.07732(12) -0.01440(14) 0.0365(5) Uani 1 1 d .
O2 O -0.25076(9) 0.01283(9) 0.07876(8) 0.0214(3) Uani 1 1 d .
N21 N -0.6667 -0.3333 0.2858(4) 0.0687(18) Uani 1 3 d S
C21 C -0.6430(7) -0.3655(7) 0.2460(6) 0.049(2) Uani 0.33 1 d P
C22 C -0.6178(10) -0.4035(9) 0.1943(7) 0.069(4) Uani 0.33 1 d P
C31 C 0.0000 0.0000 0.0000 0.104(5) Uani 1 6 d S
C32 C 0.0000 0.0000 0.0899(14) 0.076(5) Uani 0.50 3 d SP
N31 N 0.0000 0.0000 0.1473(12) 0.083(5) Uani 0.50 3 d SP
O11 O -0.3473(5) -0.3633(5) 0.2230(5) 0.090(2) Uiso 0.50 1 d P
O12 O -0.3331(9) -0.4125(9) 0.2097(8) 0.092(4) Uiso 0.33 1 d P
O13 O -0.3354(10) -0.3333 0.1667 0.073(5) Uiso 0.25 2 d SP
O14 O -0.3338(8) -0.4946(8) 0.2429(8) 0.090(4) Uiso 0.33 1 d P
O15 O -0.3312(7) -0.4501(7) 0.3061(7) 0.057(3) Uiso 0.25 1 d P
O16 O 0.0953(10) -0.0417(10) 0.1372(10) 0.089(5) Uiso 0.25 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 -0.0001 0.0005 '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 0.0005 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.2305 0.4105 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo 0.0283 1.8734 '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 123.3(2) . .
N2 C1 H1 118.3 . .
C2 C1 H1 118.3 . .
C1 C2 C3 120.0(3) . .
C1 C2 H2 120.0 . .
C3 C2 H2 120.0 . .
C2 C3 C4 116.6(2) . .
C2 C3 C6 120.3(3) . 18
C4 C3 C6 123.0(3) . 18
C5 C4 C3 119.5(2) . .
C5 C4 H4 120.2 . .
C3 C4 H4 120.2 . .
N2 C5 C4 123.8(2) . .
N2 C5 H5 118.1 . .
C4 C5 H5 118.1 . .
C7 C6 C3 124.8(3) . 18_445
C7 C6 H6 117.6 . .
C3 C6 H6 117.6 18_445 .
C6 C7 C8 125.0(3) . .
C6 C7 H7 117.5 . .
C8 C7 H7 117.5 . .
C9 C8 C12 117.22(19) . .
C9 C8 C7 119.5(2) . .
C12 C8 C7 123.3(2) . .
C10 C9 C8 119.5(2) . .
C10 C9 H9 120.2 . .
C8 C9 H9 120.2 . .
N1 C10 C9 123.3(2) . .
N1 C10 H10 118.4 . .
C9 C10 H10 118.4 . .
N1 C11 C12 122.5(2) . .
N1 C11 H11 118.7 . .
C12 C11 H11 118.7 . .
C11 C12 C8 119.8(2) . .
C11 C12 H12 120.1 . .
C8 C12 H12 120.1 . .
O1 Mo1 O1 110.30(15) . 4
O1 Mo1 O2 108.77(10) . 4
O1 Mo1 O2 110.17(10) 4 4
O1 Mo1 O2 110.17(10) . .
O1 Mo1 O2 108.77(10) 4 .
O2 Mo1 O2 108.65(11) 4 .
C10 N1 C11 117.58(18) . .
C10 N1 Ni1 123.61(14) . .
C11 N1 Ni1 118.45(15) . .
C5 N2 C1 116.8(2) . .
C5 N2 Ni1 119.42(16) . .
C1 N2 Ni1 123.82(15) . .
O2 Ni1 O2 177.93(10) . 12_455
O2 Ni1 N2 89.09(7) . .
O2 Ni1 N2 89.44(7) 12_455 .
O2 Ni1 N2 89.44(7) . 12_455
O2 Ni1 N2 89.09(7) 12_455 12_455
N2 Ni1 N2 89.30(11) . 12_455
O2 Ni1 N1 89.02(7) . .
O2 Ni1 N1 92.53(7) 12_455 .
N2 Ni1 N1 93.91(7) . .
N2 Ni1 N1 176.42(7) 12_455 .
O2 Ni1 N1 92.53(7) . 12_455
O2 Ni1 N1 89.02(7) 12_455 12_455
N2 Ni1 N1 176.42(7) . 12_455
N2 Ni1 N1 93.91(7) 12_455 12_455
N1 Ni1 N1 82.93(9) . 12_455
Mo1 O2 Ni1 170.25(10) . .
C21 N21 C21 90.5(8) 2_455 3_445
C21 N21 C21 90.5(8) 2_455 .
C21 N21 C21 90.5(8) 3_445 .
N21 C21 C22 176.0(12) . .
C22 C21 C21 133.4(10) . 2_455
C22 C21 C21 131.6(11) . 3_445
C32 C31 C32 180.000(1) . 4
N31 C32 C31 180.000(1) . .
O13 O11 O12 102.3(13) . .
O11 O13 O11 173(2) 10_445 .
O15 O14 O16 150.3(14) . 12_445
O15 O15 O14 140.8(8) 17_445 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.345(3) .
C1 C2 1.376(3) .
C1 H1 0.9500 .
C2 C3 1.398(4) .
C2 H2 0.9500 .
C3 C4 1.401(4) .
C3 C6 1.463(4) 18
C4 C5 1.376(3) .
C4 H4 0.9500 .
C5 N2 1.341(3) .
C5 H5 0.9500 .
C6 C7 1.329(4) .
C6 C3 1.463(4) 18_445
C6 H6 0.9500 .
C7 C8 1.466(3) .
C7 H7 0.9500 .
C8 C9 1.398(3) .
C8 C12 1.399(4) .
C9 C10 1.378(3) .
C9 H9 0.9500 .
C10 N1 1.343(3) .
C10 H10 0.9500 .
C11 N1 1.353(3) .
C11 C12 1.383(3) .
C11 H11 0.9500 .
C12 H12 0.9500 .
Mo1 O1 1.7492(19) .
Mo1 O1 1.7492(19) 4
Mo1 O2 1.7657(16) 4
Mo1 O2 1.7657(16) .
N1 Ni1 2.1172(17) .
N2 Ni1 2.1080(18) .
Ni1 O2 2.0294(16) .
Ni1 O2 2.0295(16) 12_455
Ni1 N2 2.1081(18) 12_455
Ni1 N1 2.1172(17) 12_455
N21 C21 1.249(13) 2_455
N21 C21 1.249(13) 3_445
N21 C21 1.249(13) .
C21 C22 1.486(18) .
C31 C32 1.62(3) .
C31 C32 1.62(3) 4
C32 N31 1.03(3) .
O11 O13 1.153(9) .
O11 O12 1.237(17) .
O13 O11 1.153(9) 10_445
O14 O15 1.456(18) .
O14 O16 1.64(2) 12_445
O15 O15 0.98(3) 17_445
O16 O14 1.64(2) 12
