#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:50:02 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178794 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/48/4104801.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_4104801
loop_
_publ_author_name
'Madhab C. Das'
'Parimal K. Bharadwaj'
_publ_section_title
;
 A Porous Coordination Polymer Exhibiting Reversible Single-Crystal to
 Single-Crystal Substitution Reactions at Mn(II) Centers by Nitrile Guest
 Molecules
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10942
_journal_page_last               10949
_journal_paper_doi               10.1021/ja9006035
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C34 H46 Mn2 N6 O15'
_chemical_formula_weight         888.65
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.000
_cell_angle_beta                 111.668(6)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   18.421(5)
_cell_length_b                   15.029(4)
_cell_length_c                   16.355(5)
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.3
_cell_volume                     4208(2)
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45  (Bruker, 2003)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13213
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_T_max  0.8944
_exptl_absorpt_correction_T_min  0.8774
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABAS 2.10 (Bruker 2003)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0637
_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)+(0.1691P)²+1.5095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.2210
_reflns_number_gt                3105
_reflns_number_total             5168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9006035_si_002_09.cif
_cod_data_source_block           complex4'
_cod_original_cell_volume        4208(3)
_cod_database_code               4104801
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Mn1 Mn 0.27585(8) 0.10828(8) 0.54667(7) 0.0340(4) Uani 1 1 d .
O4 O 0.2868(4) -0.0242(4) 0.1638(4) 0.0334(15) Uani 1 1 d .
O3 O 0.2595(4) 0.0444(4) 0.0363(4) 0.0375(16) Uani 1 1 d .
O1 O 0.1971(4) 0.2662(4) 0.3921(3) 0.0380(14) Uani 1 1 d .
O2 O 0.2535(4) 0.1331(4) 0.4124(3) 0.0385(13) Uani 1 1 d .
C2 C 0.2250(5) 0.2018(6) 0.2738(5) 0.0357(17) Uani 1 1 d .
N1 N 0.1823(5) 0.3559(5) 0.0858(5) 0.0328(17) Uani 1 1 d .
NH1 H 0.1904 0.3570 0.0372 0.039 Uiso 1 1 calc R
N2 N -0.0959(4) 0.4094(5) 0.0683(4) 0.0349(16) Uani 1 1 d .
C4 C 0.2018(5) 0.2802(6) 0.1376(5) 0.0267(17) Uani 1 1 d .
C7 C 0.2665(5) 0.0443(6) 0.1167(5) 0.0330(18) Uani 1 1 d .
C1 C 0.2468(5) 0.1263(5) 0.2403(5) 0.0392(18) Uani 1 1 d .
H1 H 0.2616 0.0751 0.2745 0.033 Uiso 1 1 calc R
C6 C 0.2465(5) 0.1275(6) 0.1552(5) 0.0326(18) Uani 1 1 d .
C3 C 0.2015(5) 0.2786(6) 0.2227(5) 0.0375(18) Uani 1 1 d .
H3 H 0.1856 0.3284 0.2454 0.034 Uiso 1 1 calc R
C8 C 0.2251(5) 0.2018(5) 0.3665(4) 0.0351(16) Uani 1 1 d .
C5 C 0.2238(6) 0.2031(6) 0.1038(5) 0.041(2) Uani 1 1 d .
H5 H 0.2231 0.2030 0.0466 0.040 Uiso 1 1 calc R
C11 C 0.0640(5) 0.4239(6) 0.0962(6) 0.0317(19) Uani 1 1 d .
OW1 O 0.1479(5) 0.1212(7) 0.5165(7) 0.0454(3) Uani 1 1 d .
C14 C 0.1488(6) 0.4326(6) 0.1110(6) 0.0321(19) Uani 1 1 d .
H14A H 0.1555 0.4837 0.0781 0.038 Uiso 1 1 calc R
H14B H 0.1775 0.4444 0.1729 0.038 Uiso 1 1 calc R
C12 C 0.0151(6) 0.3652(8) 0.0357(8) 0.035(3) Uani 1 1 d .
H12 H 0.0350 0.3288 0.0030 0.063 Uiso 1 1 calc R
C10 C 0.0292(7) 0.4759(9) 0.1394(7) 0.042(3) Uani 1 1 d .
H10 H 0.0587 0.5174 0.1803 0.068 Uiso 1 1 calc R
C9 C -0.0497(7) 0.4674(9) 0.1229(7) 0.042(3) Uani 1 1 d .
H9 H -0.0716 0.5054 0.1524 0.066 Uiso 1 1 calc R
C13 C -0.0626(6) 0.3601(8) 0.0235(8) 0.035(3) Uani 1 1 d .
H13 H -0.0939 0.3203 -0.0182 0.059 Uiso 1 1 calc R
N3 N 0.3929(13) 0.328(2) 0.2398(18) 0.054(8) Uani 1 1 d .
C17 C 0.3924(14) 0.333(3) 0.158(2) 0.061(7) Uani 1 1 d .
H17 H 0.3792 0.3869 0.1286 0.095 Uiso 1 1 calc R
C15 C 0.4136(19) 0.243(3) 0.285(4) 0.050 Uani 1 1 d .
H15A H 0.4115 0.2473 0.3422 0.099 Uiso 1 1 calc R
H15B H 0.4656 0.2267 0.2897 0.099 Uiso 1 1 calc R
H15C H 0.3775 0.1982 0.2514 0.099 Uiso 1 1 calc R
C16 C 0.3714(19) 0.405(3) 0.281(4) 0.059(6) Uani 1 1 d .
H16A H 0.3744 0.3890 0.3388 0.088 Uiso 1 1 calc R
H16B H 0.3191 0.4228 0.2460 0.088 Uiso 1 1 calc R
H16C H 0.4067 0.4531 0.2846 0.088 Uiso 1 1 calc R
O5 O 0.409(3) 0.269(5) 0.119(3) 0.045(10) Uani 1 1 d .
OW2 O -0.0149(9) 0.1047(11) 0.4156(9) 0.046 Uani 1 1 d .
OW3 O 0.0000 0.1340(4) 0.2500 0.040 Uani 1 2 d S
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'
N N 0.0061 0.0033 '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'
Mn Mn 0.3368 0.7283 '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
O1 Mn1 O2 104.9(2) 7_556 .
O1 Mn1 OW1 94.2(3) 7_556 .
O2 Mn1 OW1 88.3(3) . .
O1 Mn1 O4 99.6(2) 7_556 6_556
O2 Mn1 O4 155.4(2) . 6_556
OW1 Mn1 O4 89.6(3) . 6_556
O1 Mn1 N2 88.9(3) 7_556 8_556
O2 Mn1 N2 88.6(2) . 8_556
OW1 Mn1 N2 176.1(3) . 8_556
O4 Mn1 N2 92.3(3) 6_556 8_556
O1 Mn1 O3 157.6(2) 7_556 6_556
O2 Mn1 O3 97.4(2) . 6_556
OW1 Mn1 O3 88.4(3) . 6_556
O4 Mn1 O3 58.1(2) 6_556 6_556
N2 Mn1 O3 89.8(3) 8_556 6_556
O1 Mn1 C7 128.5(2) 7_556 6_556
O2 Mn1 C7 126.5(2) . 6_556
OW1 Mn1 C7 86.4(3) . 6_556
O4 Mn1 C7 28.9(2) 6_556 6_556
N2 Mn1 C7 93.6(3) 8_556 6_556
O3 Mn1 C7 29.3(2) 6_556 6_556
C7 O4 Mn1 91.4(5) . 6
C7 O3 Mn1 87.8(5) . 6
C8 O1 Mn1 143.6(6) . 7_556
C8 O2 Mn1 129.6(5) . .
C1 C2 C3 120.9(7) . .
C1 C2 C8 120.2(7) . .
C3 C2 C8 118.9(7) . .
C4 N1 C14 121.7(7) . .
C4 N1 NH1 119.2 . .
C14 N1 NH1 119.2 . .
C9 N2 C13 115.3(9) . .
C9 N2 Mn1 124.0(7) . 8_455
C13 N2 Mn1 120.7(6) . 8_455
N1 C4 C3 122.0(7) . .
N1 C4 C5 118.9(7) . .
C3 C4 C5 119.1(7) . .
O4 C7 O3 121.9(7) . .
O4 C7 C6 119.2(7) . .
O3 C7 C6 118.9(7) . .
O4 C7 Mn1 59.6(4) . 6
O3 C7 Mn1 62.8(4) . 6
C6 C7 Mn1 169.7(6) . 6
C2 C1 C6 119.4(7) . .
C2 C1 H1 120.3 . .
C6 C1 H1 120.3 . .
C5 C6 C1 120.5(8) . .
C5 C6 C7 119.7(7) . .
C1 C6 C7 119.7(7) . .
C4 C3 C2 119.8(7) . .
C4 C3 H3 120.1 . .
C2 C3 H3 120.1 . .
O1 C8 O2 124.6(6) . .
O1 C8 C2 119.4(7) . .
O2 C8 C2 116.1(7) . .
C6 C5 C4 120.3(7) . .
C6 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
C10 C11 C12 115.5(9) . .
C10 C11 C14 121.9(9) . .
C12 C11 C14 122.6(8) . .
N1 C14 C11 114.6(8) . .
N1 C14 H14A 108.6 . .
C11 C14 H14A 108.6 . .
N1 C14 H14B 108.6 . .
C11 C14 H14B 108.6 . .
H14A C14 H14B 107.6 . .
C13 C12 C11 120.6(9) . .
C13 C12 H12 119.7 . .
C11 C12 H12 119.7 . .
C11 C10 C9 120.5(9) . .
C11 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
N2 C9 C10 124.4(10) . .
N2 C9 H9 117.8 . .
C10 C9 H9 117.8 . .
N2 C13 C12 123.6(9) . .
N2 C13 H13 118.2 . .
C12 C13 H13 118.2 . .
C17 N3 C16 121(2) . .
C17 N3 C15 117(3) . .
C16 N3 C15 122(4) . .
O5 C17 N3 124(3) . .
O5 C17 H17 118.0 . .
N3 C17 H17 118.0 . .
N3 C15 H15A 109.5 . .
N3 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
N3 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N3 C16 H16A 109.5 . .
N3 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
N3 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 2.107(6) 7_556
Mn1 O2 2.112(5) .
Mn1 OW1 2.230(8) .
Mn1 O4 2.241(6) 6_556
Mn1 N2 2.272(8) 8_556
Mn1 O3 2.312(7) 6_556
Mn1 C7 2.597(8) 6_556
O4 C7 1.257(10) .
O4 Mn1 2.241(6) 6
O3 C7 1.273(9) .
O3 Mn1 2.312(7) 6
O1 C8 1.240(9) .
O1 Mn1 2.107(6) 7_556
O2 C8 1.270(9) .
C2 C1 1.382(11) .
C2 C3 1.396(11) .
C2 C8 1.517(9) .
N1 C4 1.385(11) .
N1 C14 1.438(11) .
N1 NH1 0.8600 .
N2 C9 1.311(12) .
N2 C13 1.338(12) .
N2 Mn1 2.272(8) 8_455
C4 C3 1.395(11) .
C4 C5 1.406(12) .
C7 C6 1.506(11) .
C7 Mn1 2.597(8) 6
C1 C6 1.391(10) .
C1 H1 0.9300 .
C6 C5 1.383(12) .
C3 H3 0.9300 .
C5 H5 0.9300 .
C11 C10 1.362(14) .
C11 C12 1.382(14) .
C11 C14 1.496(13) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C12 C13 1.373(15) .
C12 H12 0.9300 .
C10 C9 1.383(16) .
C10 H10 0.9300 .
C9 H9 0.9300 .
C13 H13 0.9300 .
N3 C17 1.34(4) .
N3 C16 1.47(6) .
N3 C15 1.46(6) .
C17 O5 1.25(8) .
C17 H17 0.9300 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
O1 Mn1 O2 C8 -31.1(8) 7_556
OW1 Mn1 O2 C8 62.7(7) .
O4 Mn1 O2 C8 147.9(7) 6_556
N2 Mn1 O2 C8 -119.6(7) 8_556
O3 Mn1 O2 C8 150.8(7) 6_556
C7 Mn1 O2 C8 147.0(7) 6_556
C14 N1 C4 C3 -10.0(13) .
C14 N1 C4 C5 171.0(9) .
Mn1 O4 C7 O3 -9.0(9) 6
Mn1 O4 C7 C6 168.2(7) 6
Mn1 O3 C7 O4 8.7(9) 6
Mn1 O3 C7 C6 -168.5(8) 6
C3 C2 C1 C6 1.1(14) .
C8 C2 C1 C6 -180.0(8) .
C2 C1 C6 C5 -0.7(14) .
C2 C1 C6 C7 -177.2(8) .
O4 C7 C6 C5 -179.7(9) .
O3 C7 C6 C5 -2.5(13) .
Mn1 C7 C6 C5 -99(3) 6
O4 C7 C6 C1 -3.2(13) .
O3 C7 C6 C1 174.1(9) .
Mn1 C7 C6 C1 77(3) 6
N1 C4 C3 C2 -177.1(8) .
C5 C4 C3 C2 1.9(14) .
C1 C2 C3 C4 -1.7(14) .
C8 C2 C3 C4 179.3(8) .
Mn1 O1 C8 O2 91.9(11) 7_556
Mn1 O1 C8 C2 -89.3(10) 7_556
Mn1 O2 C8 O1 -7.8(13) .
Mn1 O2 C8 C2 173.4(5) .
C1 C2 C8 O1 -171.9(8) .
C3 C2 C8 O1 7.1(12) .
C1 C2 C8 O2 6.9(12) .
C3 C2 C8 O2 -174.0(8) .
C1 C6 C5 C4 0.9(14) .
C7 C6 C5 C4 177.4(9) .
N1 C4 C5 C6 177.5(8) .
C3 C4 C5 C6 -1.5(14) .
C4 N1 C14 C11 -77.1(10) .
C10 C11 C14 N1 159.4(9) .
C12 C11 C14 N1 -23.1(13) .
C10 C11 C12 C13 -1.5(17) .
C14 C11 C12 C13 -179.2(10) .
C12 C11 C10 C9 1.0(17) .
C14 C11 C10 C9 178.6(10) .
C13 N2 C9 C10 -4.0(18) .
Mn1 N2 C9 C10 177.0(10) 8_455
C11 C10 C9 N2 2(2) .
C9 N2 C13 C12 3.3(17) .
Mn1 N2 C13 C12 -177.6(10) 8_455
C11 C12 C13 N2 -1(2) .
C16 N3 C17 O5 -178(4) .
C15 N3 C17 O5 0(5) .
