#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/77/4117736.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_4117736
loop_
_publ_author_name
'Masaaki Sadakiyo'
'Hisashi Ōkawa'
'Akihito Shigematsu'
'Masaaki Ohba'
'Teppei Yamada'
'Hiroshi Kitagawa'
_publ_section_title
;
 Promotion of Low-Humidity Proton Conduction by Controlling Hydrophilicity
 in Layered Metal-Organic Frameworks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5472
_journal_page_last               5475
_journal_paper_doi               10.1021/ja300122r
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C20 H30 Cr Mn N O14 '
_chemical_formula_sum            'C20 H30 Cr Mn N O14'
_chemical_formula_weight         615.39
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      161
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_audit_creation_date             2009-07-16
_audit_creation_method           'by CrystalStructure 3.8.0'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            6
_cell_length_a                   9.3928(13)
_cell_length_b                   9.3928(13)
_cell_length_c                   51.0080(13)
_cell_measurement_reflns_used    2449
_cell_measurement_temperature    100.1
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      2.40
_cell_volume                     3897.3(8)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8.0'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD-detector'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode with a mirror focusing unit'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            4750
_diffrn_reflns_theta_full        23.33
_diffrn_reflns_theta_max         23.33
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  0.9714
_exptl_absorpt_correction_T_min  0.7331
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       prism
_exptl_crystal_F_000             1908.00
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.27
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  623 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.11(7)
_refine_ls_extinction_coef       0.00018(9)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    none
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1261
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0591P)²+20.8923P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1344
_reflns_number_gt                1186
_reflns_number_total             1261
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ja300122r_si_002.cif
_cod_data_source_block           '_[N(Bu)3(etac)][MnCr(ox)3]'
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_original_formula_sum        'C20 H30 Cr Mn N O14 '
_cod_database_code               4117736
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -Y,+X-Y,+Z
3 -X+Y,-X,+Z
4 -X+Y,+Y,1/2+Z
5 +X,+X-Y,1/2+Z
6 -Y,-X,1/2+Z
7 2/3+X,1/3+Y,1/3+Z
8 2/3-Y,1/3+X-Y,1/3+Z
9 2/3-X+Y,1/3-X,1/3+Z
10 2/3-X+Y,1/3+Y,5/6+Z
11 2/3+X,1/3+X-Y,5/6+Z
12 2/3-Y,1/3-X,5/6+Z
13 1/3+X,2/3+Y,2/3+Z
14 1/3-Y,2/3+X-Y,2/3+Z
15 1/3-X+Y,2/3-X,2/3+Z
16 1/3-X+Y,2/3+Y,1/6+Z
17 1/3+X,2/3+X-Y,1/6+Z
18 1/3-Y,2/3-X,1/6+Z
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
Mn(1) Mn 0.6667 0.3333 0.53785(3) 0.0530(7) Uani 1.00 3 d S
Cr(1) Cr 0.3333 0.6667 0.53814(3) 0.0418(6) Uani 1.00 3 d S
O(1) O 0.5055(6) 0.6559(6) 0.51676(11) 0.0469(13) Uani 1.00 1 d .
O(2) O 0.3440(6) 0.4987(5) 0.55928(9) 0.0444(13) Uani 1.00 1 d .
O(3) O 0.6400(5) 0.5209(6) 0.51544(11) 0.0473(12) Uani 1.00 1 d .
O(4) O 0.4852(6) 0.3597(6) 0.56001(11) 0.0538(14) Uani 1.00 1 d .
O(5) O 0.242(4) 0.666(5) 0.7224(5) 0.290(15) Uiso 0.67 1 d P
N(1) N 0.3333 0.6667 0.6444(4) 0.110(4) Uani 1.00 3 d S
C(1) C 0.5402(9) 0.5531(9) 0.52513(16) 0.0485(19) Uani 1.00 1 d .
C(2) C 0.4498(7) 0.4601(7) 0.55031(17) 0.0384(16) Uani 1.00 1 d .
C(3) C 0.345(6) 0.748(5) 0.6707(8) 0.134(14) Uiso 0.33 1 d P
C(4) C 0.3333 0.6667 0.6931(10) 0.23(2) Uiso 1.00 3 d SP
C(5) C 0.470(4) 0.636(4) 0.6258(6) 0.288(13) Uiso 1.00 1 d .
C(6) C 0.625(6) 0.673(4) 0.6387(9) 0.35(2) Uiso 1.00 1 d .
C(7) C 0.708(3) 0.713(4) 0.6132(6) 0.133(9) Uiso 0.50 1 d P
C(8) C 0.663(3) 0.576(2) 0.6173(5) 0.105(6) Uiso 0.50 1 d P
C(9) C 0.828(3) 0.680(4) 0.6161(5) 0.268(12) Uiso 1.00 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 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cr Cr 0.321 0.624
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Mn Mn 0.337 0.728
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 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_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O(3) Mn(1) O(3) 95.8(2) yes . 2_655
O(3) Mn(1) O(3) 95.8(2) yes . 3_665
O(3) Mn(1) O(4) 76.7(2) yes . .
O(3) Mn(1) O(4) 168.67(18) yes . 2_655
O(3) Mn(1) O(4) 93.4(2) yes . 3_665
O(3) Mn(1) O(3) 95.82(19) yes 2_655 3_665
O(3) Mn(1) O(4) 93.4(2) yes 2_655 .
O(3) Mn(1) O(4) 76.7(2) yes 2_655 2_655
O(3) Mn(1) O(4) 168.7(2) yes 2_655 3_665
O(3) Mn(1) O(4) 168.68(18) yes 3_665 .
O(3) Mn(1) O(4) 93.4(2) yes 3_665 2_655
O(3) Mn(1) O(4) 76.7(2) yes 3_665 3_665
O(4) Mn(1) O(4) 95.1(2) yes . 2_655
O(4) Mn(1) O(4) 95.1(2) yes . 3_665
O(4) Mn(1) O(4) 95.1(2) yes 2_655 3_665
O(1) Cr(1) O(1) 93.0(2) yes . 2_665
O(1) Cr(1) O(1) 92.9(2) yes . 3_565
O(1) Cr(1) O(2) 83.7(2) yes . .
O(1) Cr(1) O(2) 91.0(2) yes . 2_665
O(1) Cr(1) O(2) 174.9(2) yes . 3_565
O(1) Cr(1) O(1) 93.0(2) yes 2_665 3_565
O(1) Cr(1) O(2) 174.9(2) yes 2_665 .
O(1) Cr(1) O(2) 83.7(2) yes 2_665 2_665
O(1) Cr(1) O(2) 91.1(2) yes 2_665 3_565
O(1) Cr(1) O(2) 91.0(2) yes 3_565 .
O(1) Cr(1) O(2) 175.0(2) yes 3_565 2_665
O(1) Cr(1) O(2) 83.7(2) yes 3_565 3_565
O(2) Cr(1) O(2) 92.5(2) yes . 2_665
O(2) Cr(1) O(2) 92.5(2) yes . 3_565
O(2) Cr(1) O(2) 92.5(2) yes 2_665 3_565
Cr(1) O(1) C(1) 112.8(4) yes . .
Cr(1) O(2) C(2) 112.7(4) yes . .
Mn(1) O(3) C(1) 113.1(5) yes . .
Mn(1) O(4) C(2) 113.7(4) yes . .
O(5) O(5) O(5) 60(3) yes 2_665 3_565
O(5) O(5) C(4) 65(2) yes 2_665 .
O(5) O(5) C(4) 64.6(19) yes 3_565 .
C(3) N(1) C(3) 48(2) yes . 2_665
C(3) N(1) C(3) 48(3) yes . 3_565
C(3) N(1) C(5) 134(2) yes . .
C(3) N(1) C(5) 95(2) yes . 2_665
C(3) N(1) C(5) 132(2) yes . 3_565
C(3) N(1) C(3) 48(3) yes 2_665 3_565
C(3) N(1) C(5) 132(3) yes 2_665 .
C(3) N(1) C(5) 134(2) yes 2_665 2_665
C(3) N(1) C(5) 95(2) yes 2_665 3_565
C(3) N(1) C(5) 95(2) yes 3_565 .
C(3) N(1) C(5) 132(2) yes 3_565 2_665
C(3) N(1) C(5) 134(2) yes 3_565 3_565
C(5) N(1) C(5) 93(2) yes . 2_665
C(5) N(1) C(5) 93(2) yes . 3_565
C(5) N(1) C(5) 93(2) yes 2_665 3_565
O(1) C(1) O(3) 125.8(7) yes . .
O(1) C(1) C(2) 116.3(8) yes . .
O(3) C(1) C(2) 117.9(8) yes . .
O(2) C(2) O(4) 126.9(7) yes . .
O(2) C(2) C(1) 114.5(7) yes . .
O(4) C(2) C(1) 118.5(7) yes . .
N(1) C(3) C(3) 66(2) yes . 2_665
N(1) C(3) C(3) 66(3) yes . 3_565
N(1) C(3) C(4) 120(3) yes . .
C(3) C(3) C(3) 60(4) yes 2_665 3_565
C(3) C(3) C(4) 63(3) yes 2_665 .
C(3) C(3) C(4) 63(3) yes 3_565 .
O(5) C(4) O(5) 51(2) yes . 2_665
O(5) C(4) O(5) 51(2) yes . 3_565
O(5) C(4) C(3) 130(3) yes . .
O(5) C(4) C(3) 125(2) yes . 2_665
O(5) C(4) C(3) 175(3) yes . 3_565
O(5) C(4) O(5) 51(2) yes 2_665 3_565
O(5) C(4) C(3) 175(2) yes 2_665 .
O(5) C(4) C(3) 130(2) yes 2_665 2_665
O(5) C(4) C(3) 125(3) yes 2_665 3_565
O(5) C(4) C(3) 125(2) yes 3_565 .
O(5) C(4) C(3) 175(3) yes 3_565 2_665
O(5) C(4) C(3) 130(2) yes 3_565 3_565
C(3) C(4) C(3) 55(3) yes . 2_665
C(3) C(4) C(3) 55(4) yes . 3_565
C(3) C(4) C(3) 55(3) yes 2_665 3_565
N(1) C(5) C(6) 116(3) yes . .
C(5) C(6) C(7) 90(3) yes . .
C(5) C(6) C(8) 92(3) yes . .
C(7) C(6) C(8) 45(2) yes . .
C(6) C(7) C(8) 73(2) yes . .
C(6) C(7) C(9) 104(3) yes . .
C(8) C(7) C(9) 66(3) yes . .
C(6) C(8) C(7) 63(2) yes . .
C(6) C(8) C(9) 97(2) yes . .
C(7) C(8) C(9) 63(2) yes . .
C(7) C(9) C(8) 51(2) yes . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_2
Mn(1) O(3) 2.217(6) yes .
Mn(1) O(3) 2.217(4) yes 2_655
Mn(1) O(3) 2.217(5) yes 3_665
Mn(1) O(4) 2.160(6) yes .
Mn(1) O(4) 2.160(6) yes 2_655
Mn(1) O(4) 2.160(4) yes 3_665
Cr(1) O(1) 1.995(6) yes .
Cr(1) O(1) 1.994(6) yes 2_665
Cr(1) O(1) 1.995(4) yes 3_565
Cr(1) O(2) 1.955(5) yes .
Cr(1) O(2) 1.955(4) yes 2_665
Cr(1) O(2) 1.954(5) yes 3_565
O(1) C(1) 1.239(12) yes .
O(2) C(2) 1.300(10) yes .
O(3) C(1) 1.224(11) yes .
O(4) C(2) 1.248(10) yes .
O(5) O(5) 1.47(8) yes 2_665
O(5) O(5) 1.47(4) yes 3_565
O(5) C(4) 1.72(5) yes .
N(1) C(5) 1.73(4) yes .
N(1) C(5) 1.73(4) yes 2_665
N(1) C(5) 1.73(3) yes 3_565
C(1) C(2) 1.547(10) yes .
C(3) C(3) 1.24(5) yes 2_665
C(3) C(3) 1.24(9) yes 3_565
C(3) C(4) 1.35(6) yes .
C(5) C(6) 1.47(7) yes .
C(6) C(7) 1.46(5) yes .
C(6) C(8) 1.57(6) yes .
C(7) C(8) 1.16(4) yes .
C(7) C(9) 1.32(6) yes .
C(8) C(9) 1.36(3) yes .
