#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:43:07 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178960 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/89/4118953.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_4118953
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            'C24 H20 Cr N4 Ni O9.17'
_chemical_formula_weight         621.82
_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                   21.1759(3)
_cell_length_b                   21.1759(3)
_cell_length_c                   17.4734(3)
_cell_measurement_temperature    228(2)
_cell_volume                     6785.66(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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12389
_diffrn_reflns_theta_full        68.12
_diffrn_reflns_theta_max         68.12
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    4.206
_exptl_absorpt_correction_T_max  0.6785
_exptl_absorpt_correction_T_min  0.5711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0484P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                2533
_reflns_number_total             2698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja309452y_si_003.cif
_cod_data_source_block           CROFOUR-1-Ni
_cod_original_cell_volume        6785.65(18)
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               4118953
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
Ni1 Ni 0.71740(3) 1.05074(3) 0.1667 0.01239(16) Uani 1 2 d S
Cr2 Cr 0.6667 1.12305(3) 0.3333 0.01648(17) Uani 1 2 d S
N1 N 0.67303(13) 0.94439(13) 0.21291(12) 0.0183(5) Uani 1 1 d .
O2 O 0.68412(12) 1.08640(12) 0.25870(11) 0.0213(4) Uani 1 1 d .
N3 N 0.81964(13) 1.08936(14) 0.21938(14) 0.0207(5) Uani 1 1 d .
C13 C 0.61653(16) 0.92061(18) 0.26137(16) 0.0223(6) Uani 1 1 d .
H13 H 0.6028 0.9541 0.2786 0.027 Uiso 1 1 calc R
C8 C 0.69098(17) 0.89572(17) 0.18808(17) 0.0245(7) Uani 1 1 d .
H8 H 0.7296 0.9111 0.1530 0.029 Uiso 1 1 calc R
C12 C 0.57770(19) 0.85012(19) 0.28703(19) 0.0276(7) Uani 1 1 d .
H12 H 0.5380 0.8359 0.3204 0.033 Uiso 1 1 calc R
O7 O 0.59590(14) 1.13235(15) 0.31423(16) 0.0391(6) Uani 1 1 d .
C1 C 0.86261(19) 1.0616(2) 0.2064(2) 0.0337(8) Uani 1 1 d .
H1 H 0.8465 1.0223 0.1721 0.040 Uiso 1 1 calc R
C6 C 0.84379(18) 1.1453(2) 0.2688(2) 0.0311(8) Uani 1 1 d .
H6 H 0.8140 1.1656 0.2789 0.037 Uiso 1 1 calc R
C4 C 0.9557(2) 1.1462(2) 0.2908(2) 0.0365(9) Uani 1 1 d .
C10 C 0.59767(19) 0.79941(17) 0.26313(18) 0.0293(7) Uani 1 1 d .
C9 C 0.6555(2) 0.8241(2) 0.2115(2) 0.0308(7) Uani 1 1 d .
H9 H 0.6703 0.7918 0.1928 0.037 Uiso 1 1 calc R
C5 C 0.9101(2) 1.1743(2) 0.3051(2) 0.0406(10) Uani 1 1 d .
H5 H 0.9245 1.2131 0.3397 0.049 Uiso 1 1 calc R
C7 C 1.0287(2) 1.1767(2) 0.3240(3) 0.0421(10) Uani 1 1 d .
H7 H 1.0575 1.1569 0.3073 0.051 Uiso 1 1 calc R
C3 C 0.9297(2) 1.0875(2) 0.2407(3) 0.0461(10) Uani 1 1 d .
H3 H 0.9578 1.0654 0.2302 0.055 Uiso 1 1 calc R
C11 C 0.5626(2) 0.72427(19) 0.2915(2) 0.0373(8) Uani 1 1 d .
H11 H 0.5792 0.6940 0.2713 0.045 Uiso 1 1 calc R
O1 O 0.6648(5) 0.5383(5) 0.3718(6) 0.095(3) Uani 0.50 1 d P
O3 O 0.6779(5) 0.6562(5) 0.4581(6) 0.097(3) Uani 0.50 1 d P
O4 O 0.6161(6) 0.3208(6) 0.4354(6) 0.065(3) Uani 0.33 1 d P
O5 O 0.6667 0.3976(7) 0.3333 0.127(7) Uani 0.50 2 d SP
O6 O 0.7117(6) 0.4708(8) 0.4695(6) 0.117(4) Uani 0.50 1 d P
O8 O 0.6647(7) 0.5761(8) 0.4526(9) 0.103(4) Uani 0.38 1 d P
O9 O 1.0000 1.0000 0.402(3) 0.21(2) Uani 0.38 3 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'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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 Ni1 O2 178.59(14) 12_455 .
O2 Ni1 N3 89.58(9) 12_455 .
O2 Ni1 N3 89.42(9) . .
O2 Ni1 N3 89.42(9) 12_455 12_455
O2 Ni1 N3 89.58(9) . 12_455
N3 Ni1 N3 89.81(14) . 12_455
O2 Ni1 N1 88.71(9) 12_455 .
O2 Ni1 N1 92.35(9) . .
N3 Ni1 N1 93.98(9) . .
N3 Ni1 N1 175.76(10) 12_455 .
O2 Ni1 N1 92.35(9) 12_455 12_455
O2 Ni1 N1 88.71(9) . 12_455
N3 Ni1 N1 175.76(10) . 12_455
N3 Ni1 N1 93.98(9) 12_455 12_455
N1 Ni1 N1 82.30(13) . 12_455
O7 Cr2 O7 109.5(2) 17_655 .
O7 Cr2 O2 110.06(13) 17_655 .
O7 Cr2 O2 109.17(13) . .
O7 Cr2 O2 109.17(13) 17_655 17_655
O7 Cr2 O2 110.06(13) . 17_655
O2 Cr2 O2 108.82(15) . 17_655
C8 N1 C13 117.4(3) . .
C8 N1 Ni1 123.35(19) . .
C13 N1 Ni1 118.5(2) . .
Cr2 O2 Ni1 173.57(15) . .
C1 N3 C6 117.2(3) . .
C1 N3 Ni1 123.6(2) . .
C6 N3 Ni1 119.2(2) . .
N1 C13 C12 123.5(3) . .
N1 C13 H13 118.2 . .
C12 C13 H13 118.2 . .
N1 C8 C9 123.0(3) . .
N1 C8 H8 118.5 . .
C9 C8 H8 118.5 . .
C13 C12 C10 119.4(3) . .
C13 C12 H12 120.3 . .
C10 C12 H12 120.3 . .
N3 C1 C3 123.3(3) . .
N3 C1 H1 118.4 . .
C3 C1 H1 118.4 . .
N3 C6 C5 122.9(3) . .
N3 C6 H6 118.5 . .
C5 C6 H6 118.5 . .
C5 C4 C3 116.6(3) . .
C5 C4 C7 123.3(3) . .
C3 C4 C7 120.1(4) . .
C9 C10 C12 116.8(3) . .
C9 C10 C11 119.9(3) . .
C12 C10 C11 123.3(3) . .
C8 C9 C10 119.8(3) . .
C8 C9 H9 120.1 . .
C10 C9 H9 120.1 . .
C6 C5 C4 120.1(3) . .
C6 C5 H5 120.0 . .
C4 C5 H5 120.0 . .
C11 C7 C4 125.6(4) 18 .
C11 C7 H7 117.2 18 .
C4 C7 H7 117.2 . .
C1 C3 C4 119.9(4) . .
C1 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C7 C11 C10 125.8(4) 18_445 .
C7 C11 H11 117.1 18_445 .
C10 C11 H11 117.1 . .
O1 O1 O8 150.3(7) 17_655 .
O8 O3 O3 115.1(10) . 6_556
O4 O4 O4 60.000(3) 2_655 3_665
O3 O8 O1 122.6(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.0457(19) 12_455
Ni1 O2 2.0458(19) .
Ni1 N3 2.106(2) .
Ni1 N3 2.106(2) 12_455
Ni1 N1 2.119(2) .
Ni1 N1 2.119(2) 12_455
Cr2 O7 1.641(3) 17_655
Cr2 O7 1.641(2) .
Cr2 O2 1.6512(19) .
Cr2 O2 1.6512(19) 17_655
N1 C8 1.337(4) .
N1 C13 1.342(4) .
N3 C1 1.326(4) .
N3 C6 1.343(4) .
C13 C12 1.370(5) .
C13 H13 0.9400 .
C8 C9 1.377(5) .
C8 H8 0.9400 .
C12 C10 1.400(5) .
C12 H12 0.9400 .
C1 C3 1.378(5) .
C1 H1 0.9400 .
C6 C5 1.374(5) .
C6 H6 0.9400 .
C4 C5 1.387(6) .
C4 C3 1.390(5) .
C4 C7 1.465(5) .
C10 C9 1.396(5) .
C10 C11 1.465(4) .
C9 H9 0.9400 .
C5 H5 0.9400 .
C7 C11 1.317(5) 18
C7 H7 0.9400 .
C3 H3 0.9400 .
C11 C7 1.317(5) 18_445
C11 H11 0.9400 .
O1 O1 1.35(2) 17_655
O1 O8 1.623(17) .
O3 O8 1.579(17) .
O3 O3 1.67(2) 6_556
O4 O4 1.672(19) 2_655
O4 O4 1.67(2) 3_665
