#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:29:39 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180184 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/80/7108043.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_7108043
loop_
_publ_author_name
'Ryosuke Miyake'
'Mitsuhiko Shionoya'
_publ_section_title
;
 Reversible structural switch in the nano-cavity of crystalline
 metallo-macrocycles with smooth ligand exchange by non-coordinating guest
 stimuli
;
_journal_name_full               Chem.Commun.
_journal_page_first              7553
_journal_paper_doi               10.1039/c2cc32857g
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C48 H108 N36 Ni4 O36'
_chemical_formula_weight         2000.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6619(12)
_cell_length_b                   14.6619(12)
_cell_length_c                   18.9721(16)
_cell_measurement_reflns_used    6857
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      2.78
_cell_volume                     4078.5(6)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 '
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14097
_diffrn_reflns_theta_full        29.09
_diffrn_reflns_theta_max         29.09
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.019
_exptl_absorpt_correction_T_max  0.9050
_exptl_absorpt_correction_T_min  0.8540
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.062(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5408
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0503P)²+3.1173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1057
_reflns_number_gt                4448
_reflns_number_total             5408
_reflns_threshold_expression     >2sigma
_cod_data_source_file            c2cc32857g.txt
_cod_data_source_block           i-4_293K
_cod_original_sg_symbol_H-M      'I-4 '
_cod_database_code               7108043
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6661(4) 1.0880(3) 0.7710(2) 0.0666(11) Uani 1 1 d . . .
H1A H 0.6735 1.1525 0.7774 0.100 Uiso 1 1 calc R . .
H1B H 0.6098 1.0687 0.7921 0.100 Uiso 1 1 calc R . .
H1C H 0.6653 1.0741 0.7216 0.100 Uiso 1 1 calc R . .
C2 C 0.7439(3) 1.0389(2) 0.8053(2) 0.0502(8) Uani 1 1 d . . .
C3 C 0.7917(3) 0.9478(2) 0.9075(2) 0.0481(7) Uani 1 1 d . . .
H3A H 0.7893 0.9710 0.9553 0.058 Uiso 1 1 calc R . .
H3B H 0.8517 0.9615 0.8887 0.058 Uiso 1 1 calc R . .
C4 C 0.7795(2) 0.84376(18) 0.90946(17) 0.0374(6) Uani 1 1 d . . .
C5 C 0.8560(3) 0.8056(2) 0.95727(18) 0.0471(8) Uani 1 1 d . . .
H5A H 0.9126 0.8368 0.9462 0.057 Uiso 1 1 calc R . .
H5B H 0.8411 0.8189 1.0060 0.057 Uiso 1 1 calc R . .
C6 C 0.6847(2) 0.8221(2) 0.93890(19) 0.0451(7) Uani 1 1 d . . .
H6A H 0.6718 0.8635 0.9775 0.054 Uiso 1 1 calc R . .
H6B H 0.6397 0.8330 0.9024 0.054 Uiso 1 1 calc R . .
C7 C 0.79072(19) 0.79830(19) 0.83746(15) 0.0325(5) Uani 1 1 d . . .
C8 C 0.8472(2) 0.7938(3) 0.71838(17) 0.0428(7) Uani 1 1 d . . .
H8A H 0.8214 0.8301 0.6806 0.051 Uiso 1 1 calc R . .
H8B H 0.8148 0.7362 0.7195 0.051 Uiso 1 1 calc R . .
C9 C 0.9491(2) 0.7749(2) 0.70151(16) 0.0383(6) Uani 1 1 d . . .
C10 C 0.9843(2) 0.8616(2) 0.6657(2) 0.0487(8) Uani 1 1 d . . .
H10A H 0.9426 0.8769 0.6277 0.058 Uiso 1 1 calc R . .
H10B H 0.9818 0.9109 0.6997 0.058 Uiso 1 1 calc R . .
C11 C 0.9482(2) 0.6934(2) 0.65112(17) 0.0408(6) Uani 1 1 d . . .
H11A H 0.9123 0.6450 0.6722 0.049 Uiso 1 1 calc R . .
H11B H 0.9179 0.7116 0.6079 0.049 Uiso 1 1 calc R . .
C12 C 0.9954(2) 0.7476(2) 0.77019(16) 0.0403(7) Uani 1 1 d . . .
N1 N 0.7235(2) 0.99535(19) 0.86528(16) 0.0474(6) Uani 1 1 d . . .
H1 H 0.6678 0.9954 0.8795 0.057 Uiso 1 1 calc R . .
N2 N 0.8700(2) 0.7075(2) 0.94963(16) 0.0460(6) Uani 1 1 d . . .
H2A H 0.8874 0.6849 0.9916 0.055 Uiso 1 1 calc R . .
H2B H 0.9161 0.6984 0.9192 0.055 Uiso 1 1 calc R . .
N3 N 0.6749(2) 0.72856(19) 0.96408(15) 0.0441(6) Uani 1 1 d . . .
H3C H 0.6161 0.7119 0.9591 0.053 Uiso 1 1 calc R . .
H3D H 0.6878 0.7275 1.0105 0.053 Uiso 1 1 calc R . .
N4 N 0.83222(18) 0.84148(19) 0.78539(14) 0.0402(6) Uani 1 1 d . . .
H4 H 0.8502 0.8969 0.7907 0.048 Uiso 1 1 calc R . .
N5 N 1.07636(19) 0.8584(2) 0.63661(16) 0.0461(6) Uani 1 1 d . . .
H5C H 1.1143 0.8720 0.6724 0.055 Uiso 1 1 calc R . .
H5D H 1.0803 0.9049 0.6058 0.055 Uiso 1 1 calc R . .
N6 N 1.03853(18) 0.65714(18) 0.63341(14) 0.0388(5) Uani 1 1 d . . .
H6C H 1.0305 0.6090 0.6046 0.047 Uiso 1 1 calc R . .
H6D H 1.0639 0.6360 0.6734 0.047 Uiso 1 1 calc R . .
N7 N 1.0526(3) 0.8068(3) 0.8005(2) 0.0733(11) Uani 1 1 d . . .
H7A H 1.0780 0.7936 0.8401 0.088 Uiso 1 1 calc R . .
H7B H 1.0640 0.8582 0.7805 0.088 Uiso 1 1 calc R . .
N1M N 0.7600(3) 0.5673(2) 1.06617(16) 0.0588(8) Uani 1 1 d D . .
N2MA N 0.5000 1.0000 0.9688(3) 0.0525(10) Uani 1 2 d SD . .
N3M N 0.5047(15) 0.4916(13) 1.0068(10) 0.040(4) Uani 0.25 1 d PDU A -1
N2MB N 0.996(4) 0.0085(18) 0.9621(10) 0.062(4) Uani 0.25 1 d PDU B -2
Ni1 Ni 0.75567(3) 0.63220(2) 0.914201(19) 0.03586(10) Uani 1 1 d . . .
O1 O 0.8214(2) 1.0373(2) 0.77925(16) 0.0648(7) Uani 1 1 d . . .
O2 O 0.76323(15) 0.71863(14) 0.82944(10) 0.0366(4) Uani 1 1 d . . .
O3 O 0.97794(19) 0.6747(2) 0.79705(14) 0.0569(6) Uani 1 1 d . . .
O1M O 0.7460(3) 0.5112(2) 1.11238(16) 0.0847(11) Uani 1 1 d . . .
O2M O 0.7569(2) 0.54131(18) 1.00176(13) 0.0636(8) Uani 1 1 d . . .
O3M O 0.7769(3) 0.6473(2) 1.08047(14) 0.0701(8) Uani 1 1 d D . .
O4MA O 0.5688(3) 1.0028(4) 0.9990(4) 0.170(3) Uani 1 1 d D . .
O5MA O 0.5000 1.0000 0.9065(4) 0.177(4) Uani 1 2 d SD . .
O9M O 0.5652(16) 0.5451(16) 1.0144(12) 0.118(7) Uani 0.25 1 d PDU A -1
O7M O 0.5093(10) 0.4267(8) 0.9695(7) 0.054(3) Uani 0.25 1 d PDU A -1
O8M O 0.4510(12) 0.4866(11) 1.0548(7) 0.072(4) Uani 0.25 1 d PDU A -1
O4MB O 0.9635(10) 0.0782(9) 0.9411(7) 0.057(3) Uani 0.25 1 d PDU B -2
O5MB O 1.0180(14) -0.0498(11) 0.9220(9) 0.095(5) Uani 0.25 1 d PDU B -2
O6MB O 0.9769(17) -0.0146(16) 1.0233(8) 0.088(6) Uani 0.25 1 d PDU B -2
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'
Ni Ni 0.3393 1.1124 '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
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
O1 C2 N1 122.3(4) . .
O1 C2 C1 122.3(4) . .
N1 C2 C1 115.3(4) . .
N1 C3 C4 114.1(3) . .
N1 C3 H3A 108.7 . .
C4 C3 H3A 108.7 . .
N1 C3 H3B 108.7 . .
C4 C3 H3B 108.7 . .
H3A C3 H3B 107.6 . .
C7 C4 C6 109.5(2) . .
C7 C4 C3 113.5(3) . .
C6 C4 C3 108.8(3) . .
C7 C4 C5 106.7(2) . .
C6 C4 C5 111.7(3) . .
C3 C4 C5 106.8(3) . .
N2 C5 C4 113.5(3) . .
N2 C5 H5A 108.9 . .
C4 C5 H5A 108.9 . .
N2 C5 H5B 108.9 . .
C4 C5 H5B 108.9 . .
H5A C5 H5B 107.7 . .
N3 C6 C4 113.9(3) . .
N3 C6 H6A 108.8 . .
C4 C6 H6A 108.8 . .
N3 C6 H6B 108.8 . .
C4 C6 H6B 108.8 . .
H6A C6 H6B 107.7 . .
O2 C7 N4 120.5(3) . .
O2 C7 C4 118.9(2) . .
N4 C7 C4 120.6(3) . .
N4 C8 C9 114.1(3) . .
N4 C8 H8A 108.7 . .
C9 C8 H8A 108.7 . .
N4 C8 H8B 108.7 . .
C9 C8 H8B 108.7 . .
H8A C8 H8B 107.6 . .
C12 C9 C11 109.4(3) . .
C12 C9 C10 116.7(3) . .
C11 C9 C10 111.9(3) . .
C12 C9 C8 107.4(2) . .
C11 C9 C8 105.0(3) . .
C10 C9 C8 105.5(3) . .
N5 C10 C9 117.0(3) . .
N5 C10 H10A 108.1 . .
C9 C10 H10A 108.1 . .
N5 C10 H10B 108.1 . .
C9 C10 H10B 108.1 . .
H10A C10 H10B 107.3 . .
N6 C11 C9 114.7(3) . .
N6 C11 H11A 108.6 . .
C9 C11 H11A 108.6 . .
N6 C11 H11B 108.6 . .
C9 C11 H11B 108.6 . .
H11A C11 H11B 107.6 . .
O3 C12 N7 121.6(3) . .
O3 C12 C9 119.9(3) . .
N7 C12 C9 118.5(3) . .
C2 N1 C3 122.8(3) . .
C2 N1 H1 118.6 . .
C3 N1 H1 118.6 . .
C5 N2 Ni1 115.8(2) . .
C5 N2 H2A 108.3 . .
Ni1 N2 H2A 108.3 . .
C5 N2 H2B 108.3 . .
Ni1 N2 H2B 108.3 . .
H2A N2 H2B 107.4 . .
C6 N3 Ni1 115.7(2) . .
C6 N3 H3C 108.3 . .
Ni1 N3 H3C 108.3 . .
C6 N3 H3D 108.3 . .
Ni1 N3 H3D 108.3 . .
H3C N3 H3D 107.4 . .
C7 N4 C8 119.3(3) . .
C7 N4 H4 120.4 . .
C8 N4 H4 120.4 . .
C10 N5 Ni1 124.1(2) . 7_566
C10 N5 H5C 106.3 . .
Ni1 N5 H5C 106.3 7_566 .
C10 N5 H5D 106.3 . .
Ni1 N5 H5D 106.3 7_566 .
H5C N5 H5D 106.4 . .
C11 N6 Ni1 118.2(2) . 7_566
C11 N6 H6C 107.8 . .
Ni1 N6 H6C 107.8 7_566 .
C11 N6 H6D 107.8 . .
Ni1 N6 H6D 107.8 7_566 .
H6C N6 H6D 107.1 . .
C12 N7 H7A 120.0 . .
C12 N7 H7B 120.0 . .
H7A N7 H7B 120.0 . .
O1M N1M O3M 121.3(3) . .
O1M N1M O2M 118.6(3) . .
O3M N1M O2M 120.1(3) . .
O4MA N2MA O4MA 120.9(9) . 2_675
O4MA N2MA O5MA 119.5(5) . .
O4MA N2MA O5MA 119.5(5) 2_675 .
O7M N3M O9M 123.8(15) . .
O7M N3M O8M 116.0(14) . .
O9M N3M O8M 115.7(13) . .
O5MB N2MB O4MB 120.6(17) . .
O5MB N2MB O6MB 118(2) . .
O4MB N2MB O6MB 117(2) . .
O2 Ni1 N3 88.15(10) . .
O2 Ni1 N6 91.96(9) . 8_646
N3 Ni1 N6 176.97(13) . 8_646
O2 Ni1 N5 85.64(10) . 8_646
N3 Ni1 N5 91.14(12) . 8_646
N6 Ni1 N5 91.88(10) 8_646 8_646
O2 Ni1 N2 83.33(10) . .
N3 Ni1 N2 87.25(13) . .
N6 Ni1 N2 89.76(11) 8_646 .
N5 Ni1 N2 168.89(12) 8_646 .
O2 Ni1 O2M 176.38(12) . .
N3 Ni1 O2M 94.31(11) . .
N6 Ni1 O2M 85.44(11) 8_646 .
N5 Ni1 O2M 96.95(13) 8_646 .
N2 Ni1 O2M 94.13(12) . .
C7 O2 Ni1 120.11(18) . .
N1M O2M Ni1 123.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.497(6) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 O1 1.240(5) .
C2 N1 1.339(5) .
C3 N1 1.459(5) .
C3 C4 1.536(4) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C7 1.529(4) .
C4 C6 1.531(5) .
C4 C5 1.548(5) .
C5 N2 1.460(5) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 N3 1.459(4) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 O2 1.245(4) .
C7 N4 1.322(4) .
C8 N4 1.467(4) .
C8 C9 1.553(4) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C12 1.523(4) .
C9 C11 1.530(5) .
C9 C10 1.530(4) .
C10 N5 1.459(4) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 N6 1.467(4) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 O3 1.211(4) .
C12 N7 1.338(5) .
N1 H1 0.8600 .
N2 Ni1 2.116(3) .
N2 H2A 0.9000 .
N2 H2B 0.9000 .
N3 Ni1 2.073(3) .
N3 H3C 0.9000 .
N3 H3D 0.9000 .
N4 H4 0.8600 .
N5 Ni1 2.097(3) 7_566
N5 H5C 0.9000 .
N5 H5D 0.9000 .
N6 Ni1 2.082(3) 7_566
N6 H6C 0.9000 .
N6 H6D 0.9000 .
N7 H7A 0.8600 .
N7 H7B 0.8600 .
N1M O1M 1.220(4) .
N1M O3M 1.228(4) .
N1M O2M 1.281(4) .
N2MA O4MA 1.161(5) .
N2MA O4MA 1.161(5) 2_675
N2MA O5MA 1.181(8) .
N3M O7M 1.188(13) .
N3M O9M 1.193(13) .
N3M O8M 1.206(13) .
N2MB O5MB 1.188(13) .
N2MB O4MB 1.198(14) .
N2MB O6MB 1.24(3) .
Ni1 O2 2.050(2) .
Ni1 N6 2.082(3) 8_646
Ni1 N5 2.097(3) 8_646
Ni1 O2M 2.130(3) .
