#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/43/4104324.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_4104324
loop_
_publ_author_name
'Tao Wu'
'Jian Zhang'
'Cong Zhou'
'Le Wang'
'Xianhui Bu'
'Pingyun Feng'
_publ_section_title
;
 Zeolite RHO-Type Net with the Lightest Elements
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6111
_journal_page_last               6113
_journal_paper_doi               10.1021/ja901725v
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C20.5 H23.5 B Cu N8'
_chemical_formula_weight         456.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           207
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 4 2 3'
_symmetry_space_group_name_H-M   'P 4 3 2'
_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            24
_cell_length_a                   26.81520(10)
_cell_length_b                   26.81520(10)
_cell_length_c                   26.81520(10)
_cell_measurement_temperature    150(2)
_cell_volume                     19281.60(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            90405
_diffrn_reflns_theta_full        24.93
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    0.943
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5676
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_coef       0.0017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         5657
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1161P)²+11.6495P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1706
_refine_ls_wR_factor_ref         0.1967
_reflns_number_gt                4713
_reflns_number_total             5657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901725v_si_002_2.cif
_cod_data_source_block           LIF-1-Cu
_cod_original_formula_sum        'C20.50 H23.50 B Cu N8'
_cod_database_code               4104324
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
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
Cu1 Cu 0.246725(18) 0.38951(2) 0.10842(2) 0.0399(2) Uani 1 1 d .
B1 B 0.0989(2) 0.40114(19) 0.24908(17) 0.0379(11) Uani 1 1 d .
N11 N 0.13353(14) 0.37414(13) 0.21157(13) 0.0388(8) Uani 1 1 d .
N12 N 0.19411(15) 0.36425(14) 0.15523(14) 0.0434(9) Uani 1 1 d .
C11 C 0.17377(16) 0.39438(16) 0.18869(16) 0.0376(9) Uani 1 1 d .
H11 H 0.1861 0.4268 0.1959 0.045 Uiso 1 1 calc R
C12 C 0.16586(19) 0.32145(16) 0.15681(18) 0.0483(11) Uani 1 1 d .
C13 C 0.12837(19) 0.32771(18) 0.19056(18) 0.0474(11) Uani 1 1 d .
H13 H 0.1031 0.3041 0.1982 0.057 Uiso 1 1 calc R
C14 C 0.1787(3) 0.2771(2) 0.1249(3) 0.083(2) Uani 1 1 d .
H14A H 0.1622 0.2473 0.1383 0.125 Uiso 1 1 calc R
H14B H 0.2149 0.2720 0.1251 0.125 Uiso 1 1 calc R
H14C H 0.1673 0.2830 0.0907 0.125 Uiso 1 1 calc R
N21 N 0.11889(13) 0.45375(13) 0.25879(13) 0.0378(8) Uani 1 1 d .
N22 N 0.12889(15) 0.53578(14) 0.25553(14) 0.0419(9) Uani 1 1 d .
C21 C 0.10088(16) 0.49775(17) 0.24294(15) 0.0373(9) Uani 1 1 d .
H21 H 0.0708 0.5010 0.2244 0.045 Uiso 1 1 calc R
C22 C 0.16803(18) 0.51529(17) 0.28199(17) 0.0436(11) Uani 1 1 d .
C23 C 0.16221(17) 0.46558(18) 0.28440(18) 0.0439(11) Uani 1 1 d .
H23 H 0.1838 0.4427 0.3007 0.053 Uiso 1 1 calc R
C24 C 0.2082(3) 0.5472(2) 0.3034(2) 0.0209(14) Uani 0.50 1 d P
H24A H 0.2331 0.5260 0.3198 0.031 Uiso 0.50 1 calc PR
H24B H 0.1937 0.5702 0.3279 0.031 Uiso 0.50 1 calc PR
H24C H 0.2241 0.5663 0.2767 0.031 Uiso 0.50 1 calc PR
N31 N 0.09758(13) 0.37363(13) 0.29994(13) 0.0369(8) Uani 1 1 d .
N32 N 0.10087(14) 0.31487(14) 0.35821(14) 0.0400(8) Uani 1 1 d .
C31 C 0.10918(16) 0.32598(16) 0.31136(15) 0.0366(9) Uani 1 1 d .
H31 H 0.1221 0.3029 0.2878 0.044 Uiso 1 1 calc R
C32 C 0.08232(17) 0.35836(17) 0.37921(16) 0.0409(10) Uani 1 1 d .
C33 C 0.08015(17) 0.39385(17) 0.34400(16) 0.0403(10) Uani 1 1 d .
H33 H 0.0687 0.4271 0.3486 0.048 Uiso 1 1 calc R
C34 C 0.0681(2) 0.3630(2) 0.43332(19) 0.0588(14) Uani 1 1 d .
H34A H 0.0532 0.3958 0.4393 0.088 Uiso 1 1 calc R
H34B H 0.0980 0.3592 0.4541 0.088 Uiso 1 1 calc R
H34C H 0.0440 0.3369 0.4418 0.088 Uiso 1 1 calc R
N41 N 0.04594(13) 0.40230(13) 0.22687(13) 0.0379(8) Uani 1 1 d .
N42 N -0.03609(14) 0.39660(14) 0.22018(14) 0.0411(9) Uani 1 1 d .
C41 C 0.00287(17) 0.39088(15) 0.24921(15) 0.0358(9) Uani 1 1 d .
H41 H 0.0007 0.3797 0.2828 0.043 Uiso 1 1 calc R
C42 C -0.01741(18) 0.41247(17) 0.17540(17) 0.0438(11) Uani 1 1 d .
C43 C 0.03249(18) 0.41584(18) 0.17886(17) 0.0461(11) Uani 1 1 d .
H43 H 0.0546 0.4257 0.1530 0.055 Uiso 1 1 calc R
C44 C -0.0509(2) 0.4232(2) 0.1313(2) 0.0613(14) Uani 1 1 d .
H44A H -0.0712 0.3938 0.1239 0.092 Uiso 1 1 calc R
H44B H -0.0305 0.4315 0.1022 0.092 Uiso 1 1 calc R
H44C H -0.0728 0.4514 0.1392 0.092 Uiso 1 1 calc R
C1 C 0.2801(3) 0.3097(3) 0.2379(3) 0.0786(19) Uani 1 1 d .
H1 H 0.2834 0.3331 0.2115 0.094 Uiso 1 1 calc R
C2 C 0.2422(3) 0.3144(3) 0.2708(3) 0.0796(19) Uani 1 1 d .
H2 H 0.2188 0.3408 0.2675 0.096 Uiso 1 1 calc R
C3 C 1.0000 0.2568(12) 0.2568(12) 0.426(11) Uiso 1 2 d SD
H3 H 1.0000 0.2819 0.2819 0.511 Uiso 1 2 calc SR
C4 C 0.9919(12) 0.2060(10) 0.2616(13) 0.426(11) Uiso 1 1 d D
H4 H 0.9863 0.1949 0.2947 0.511 Uiso 1 1 calc R
C5 C 0.9907(12) 0.1666(12) 0.2235(9) 0.426(11) Uiso 1 1 d D
H5 H 0.9826 0.1342 0.2356 0.511 Uiso 1 1 calc R
C6 C 1.0000 0.1697(12) 0.1697(12) 0.426(11) Uiso 1 2 d SD
H6 H 1.0000 0.1446 0.1446 0.511 Uiso 1 2 calc SR
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'
B B 0.0013 0.0007 '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'
Cu Cu 0.3201 1.2651 '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
N12 Cu1 N32 123.94(15) . 9
N12 Cu1 N42 112.00(16) . 21
N32 Cu1 N42 104.75(15) 9 21
N12 Cu1 N22 103.80(15) . 22_565
N32 Cu1 N22 108.79(15) 9 22_565
N42 Cu1 N22 101.33(15) 21 22_565
N21 B1 N41 111.7(4) . .
N21 B1 N11 109.3(3) . .
N41 B1 N11 108.1(3) . .
N21 B1 N31 107.3(3) . .
N41 B1 N31 109.2(3) . .
N11 B1 N31 111.2(4) . .
C11 N11 C13 104.9(4) . .
C11 N11 B1 125.8(4) . .
C13 N11 B1 129.0(4) . .
C11 N12 C12 105.1(4) . .
C11 N12 Cu1 120.5(3) . .
C12 N12 Cu1 133.5(3) . .
N12 C11 N11 113.0(4) . .
N12 C11 H11 123.5 . .
N11 C11 H11 123.5 . .
C13 C12 N12 108.9(4) . .
C13 C12 C14 130.0(5) . .
N12 C12 C14 121.1(5) . .
C12 C13 N11 108.0(4) . .
C12 C13 H13 126.0 . .
N11 C13 H13 126.0 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C21 N21 C23 104.9(4) . .
C21 N21 B1 129.0(4) . .
C23 N21 B1 126.0(4) . .
C21 N22 C22 105.0(4) . .
C21 N22 Cu1 124.5(3) . 22_565
C22 N22 Cu1 129.7(3) . 22_565
N22 C21 N21 113.3(4) . .
N22 C21 H21 123.3 . .
N21 C21 H21 123.3 . .
C23 C22 N22 109.3(4) . .
C23 C22 C24 129.4(5) . .
N22 C22 C24 121.3(4) . .
C22 C23 N21 107.5(4) . .
C22 C23 H23 126.3 . .
N21 C23 H23 126.3 . .
C22 C24 H24A 109.5 . .
C22 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C22 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C31 N31 C33 104.8(3) . .
C31 N31 B1 130.1(4) . .
C33 N31 B1 124.9(4) . .
C31 N32 C32 105.0(4) . .
C31 N32 Cu1 125.9(3) . 5
C32 N32 Cu1 128.9(3) . 5
N32 C31 N31 113.2(4) . .
N32 C31 H31 123.4 . .
N31 C31 H31 123.4 . .
C33 C32 N32 109.0(4) . .
C33 C32 C34 127.5(4) . .
N32 C32 C34 123.4(4) . .
C32 C33 N31 108.0(4) . .
C32 C33 H33 126.0 . .
N31 C33 H33 126.0 . .
C32 C34 H34A 109.5 . .
C32 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
C32 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
C41 N41 C43 104.6(4) . .
C41 N41 B1 128.2(4) . .
C43 N41 B1 127.2(4) . .
C41 N42 C42 105.4(4) . .
C41 N42 Cu1 122.0(3) . 23
C42 N42 Cu1 132.2(3) . 23
N42 C41 N41 113.3(4) . .
N42 C41 H41 123.4 . .
N41 C41 H41 123.4 . .
C43 C42 N42 108.9(4) . .
C43 C42 C44 129.2(5) . .
N42 C42 C44 121.8(4) . .
C42 C43 N41 107.8(4) . .
C42 C43 H43 126.1 . .
N41 C43 H43 126.1 . .
C42 C44 H44A 109.5 . .
C42 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
C42 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
C2 C1 C2 120.7(8) . 9
C2 C1 H1 119.6 . .
C2 C1 H1 119.6 9 .
C1 C2 C1 119.3(8) . 5
C1 C2 H2 120.4 . .
C1 C2 H2 120.4 5 .
C4 C3 C4 102(5) 18_755 .
C4 C3 H3 129.1 18_755 .
C4 C3 H3 129.1 . .
C3 C4 C5 130(4) . .
C3 C4 H4 114.8 . .
C5 C4 H4 114.8 . .
C6 C5 C4 130(4) . .
C6 C5 H5 115.2 . .
C4 C5 H5 115.2 . .
C5 C6 C5 98(4) . 18_755
C5 C6 H6 131.0 . .
C5 C6 H6 131.0 18_755 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N12 2.006(4) .
Cu1 N32 2.021(4) 9
Cu1 N42 2.075(4) 21
Cu1 N22 2.091(4) 22_565
B1 N21 1.531(6) .
B1 N41 1.540(6) .
B1 N11 1.549(6) .
B1 N31 1.551(6) .
N11 C11 1.355(6) .
N11 C13 1.373(6) .
N12 C11 1.325(6) .
N12 C12 1.376(6) .
C11 H11 0.9500 .
C12 C13 1.363(7) .
C12 C14 1.504(7) .
C13 H13 0.9500 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
N21 C21 1.344(6) .
N21 C23 1.386(6) .
N22 C21 1.311(6) .
N22 C22 1.381(6) .
N22 Cu1 2.091(4) 22_565
C21 H21 0.9500 .
C22 C23 1.344(7) .
C22 C24 1.490(7) .
C23 H23 0.9500 .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
N31 C31 1.350(6) .
N31 C33 1.381(6) .
N32 C31 1.310(6) .
N32 C32 1.387(6) .
N32 Cu1 2.021(4) 5
C31 H31 0.9500 .
C32 C33 1.342(6) .
C32 C34 1.505(7) .
C33 H33 0.9500 .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
N41 C41 1.337(6) .
N41 C43 1.385(6) .
N42 C41 1.312(6) .
N42 C42 1.369(6) .
N42 Cu1 2.075(4) 23
C41 H41 0.9500 .
C42 C43 1.345(7) .
C42 C44 1.513(7) .
C43 H43 0.9500 .
C44 H44A 0.9800 .
C44 H44B 0.9800 .
C44 H44C 0.9800 .
C1 C2 1.352(8) .
C1 C2 1.394(8) 9
C1 H1 0.9500 .
C2 C1 1.394(8) 5
C2 H2 0.9500 .
C3 C4 1.386(17) 18_755
C3 C4 1.386(17) .
C3 H3 0.9500 .
C4 C5 1.470(17) .
C4 H4 0.9500 .
C5 C6 1.468(18) .
C5 H5 0.9500 .
C6 C5 1.468(18) 18_755
C6 H6 0.9500 .
