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#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/11/7031120.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_7031120
loop_
_publ_author_name
'Xiao, Hong-Ping'
'Zhou, Jian'
'Wang, Xiao-Li'
'Zou, Hua-Hong'
'Zhao, Rong-Qing'
'Xiao, Hong'
_publ_section_title
;
 Solvothermal syntheses and characterizations of three new holmium
 selenidostannates(iv): a rare example of adamantane-like [Sn4Se10](4-)
 selenidostannate(iv) with lanthanide complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12306
_journal_page_last               12312
_journal_paper_doi               10.1039/c4dt00972j
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C16 H54 Ho2 N12 O2, Se6 Sn2'
_chemical_formula_sum            'C16 H54 Ho2 N12 O2 Se6 Sn2'
_chemical_formula_weight         1487.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.1380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0096(6)
_cell_length_b                   11.7181(6)
_cell_length_c                   13.7717(7)
_cell_measurement_temperature    100(2)
_cell_volume                     1913.49(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13479
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    11.121
_exptl_absorpt_correction_T_max  0.3313
_exptl_absorpt_correction_T_min  0.1808
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'optimized using Stoe X-shape'
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    2.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3364
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0215
_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)+(0.0280P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0529
_reflns_number_gt                3057
_reflns_number_total             3364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00972j3.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7031119--7031121.cif.'
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7031120
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ho1 Ho 0.475756(14) 0.418188(15) 0.611311(12) 0.01238(7) Uani 1 1 d .
Sn1 Sn 0.50550(2) 0.02112(2) 0.872515(18) 0.01444(8) Uani 1 1 d .
Se1 Se 0.66822(3) 0.12188(4) 0.82328(3) 0.01895(11) Uani 1 1 d .
Se2 Se 0.42335(3) 0.13921(3) 1.00535(3) 0.01823(10) Uani 1 1 d .
Se3 Se 0.36123(3) -0.02355(3) 0.73035(3) 0.01900(11) Uani 1 1 d .
O1W O 0.4190(2) 0.4486(2) 0.45120(19) 0.0172(6) Uani 1 1 d D
N1 N 0.2726(3) 0.3525(3) 0.5833(2) 0.0175(7) Uani 1 1 d .
H1A H 0.2403 0.3743 0.6350 0.021 Uiso 1 1 calc R
H1B H 0.2359 0.3880 0.5296 0.021 Uiso 1 1 calc R
N2 N 0.4578(3) 0.2075(3) 0.5664(2) 0.0161(7) Uani 1 1 d .
H2C H 0.4717 0.1650 0.6223 0.019 Uiso 1 1 calc R
N3 N 0.6625(3) 0.3122(3) 0.6225(2) 0.0207(8) Uani 1 1 d .
H3A H 0.7129 0.3594 0.6018 0.025 Uiso 1 1 calc R
H3B H 0.6874 0.2966 0.6862 0.025 Uiso 1 1 calc R
N4 N 0.4488(3) 0.3290(3) 0.7738(2) 0.0210(8) Uani 1 1 d .
H4A H 0.3760 0.3084 0.7697 0.025 Uiso 1 1 calc R
H4B H 0.4905 0.2649 0.7824 0.025 Uiso 1 1 calc R
N5 N 0.5895(3) 0.5204(3) 0.7614(2) 0.0179(7) Uani 1 1 d .
H5C H 0.6623 0.5221 0.7506 0.022 Uiso 1 1 calc R
N6 N 0.3692(3) 0.5836(3) 0.6647(3) 0.0199(8) Uani 1 1 d .
H6A H 0.3522 0.6310 0.6130 0.024 Uiso 1 1 calc R
H6B H 0.3036 0.5572 0.6797 0.024 Uiso 1 1 calc R
C1 C 0.2576(3) 0.2281(3) 0.5699(3) 0.0200(9) Uani 1 1 d .
H1C H 0.1826 0.2125 0.5347 0.024 Uiso 1 1 calc R
H1D H 0.2647 0.1914 0.6337 0.024 Uiso 1 1 calc R
C2 C 0.3438(3) 0.1803(4) 0.5137(3) 0.0194(9) Uani 1 1 d .
H2A H 0.3347 0.0983 0.5074 0.023 Uiso 1 1 calc R
H2B H 0.3338 0.2131 0.4482 0.023 Uiso 1 1 calc R
C3 C 0.5459(3) 0.1843(4) 0.5056(3) 0.0203(9) Uani 1 1 d .
H3C H 0.5357 0.2343 0.4487 0.024 Uiso 1 1 calc R
H3D H 0.5398 0.1060 0.4825 0.024 Uiso 1 1 calc R
C4 C 0.6611(3) 0.2040(4) 0.5660(3) 0.0210(9) Uani 1 1 d .
H4C H 0.6798 0.1408 0.6111 0.025 Uiso 1 1 calc R
H4D H 0.7174 0.2074 0.5228 0.025 Uiso 1 1 calc R
C5 C 0.4787(4) 0.4015(4) 0.8614(3) 0.0229(9) Uani 1 1 d .
H5A H 0.4851 0.3552 0.9205 0.028 Uiso 1 1 calc R
H5B H 0.4205 0.4583 0.8639 0.028 Uiso 1 1 calc R
C6 C 0.5907(4) 0.4599(4) 0.8560(3) 0.0234(10) Uani 1 1 d .
H6C H 0.6069 0.5141 0.9096 0.028 Uiso 1 1 calc R
H6D H 0.6503 0.4033 0.8638 0.028 Uiso 1 1 calc R
C7 C 0.5520(3) 0.6409(4) 0.7610(3) 0.0215(9) Uani 1 1 d .
H7A H 0.5786 0.6810 0.7075 0.026 Uiso 1 1 calc R
H7B H 0.5855 0.6770 0.8221 0.026 Uiso 1 1 calc R
C8 C 0.4253(4) 0.6516(4) 0.7494(3) 0.0231(9) Uani 1 1 d .
H8A H 0.3998 0.6254 0.8090 0.028 Uiso 1 1 calc R
H8B H 0.4041 0.7312 0.7397 0.028 Uiso 1 1 calc R
H1W H 0.354(2) 0.433(4) 0.425(3) 0.026(13) Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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
O1W Ho1 O1W 67.36(11) . 3_666
O1W Ho1 N6 94.38(11) . .
O1W Ho1 N6 85.39(11) 3_666 .
O1W Ho1 N1 76.23(10) . .
O1W Ho1 N1 137.35(10) 3_666 .
N6 Ho1 N1 75.76(11) . .
O1W Ho1 N4 151.16(10) . .
O1W Ho1 N4 141.01(10) 3_666 .
N6 Ho1 N4 85.25(12) . .
N1 Ho1 N4 75.75(11) . .
O1W Ho1 N2 85.06(10) . .
O1W Ho1 N2 127.39(10) 3_666 .
N6 Ho1 N2 142.84(11) . .
N1 Ho1 N2 68.01(10) . .
N4 Ho1 N2 78.28(11) . .
O1W Ho1 N3 105.40(11) . .
O1W Ho1 N3 79.62(11) 3_666 .
N6 Ho1 N3 148.04(11) . .
N1 Ho1 N3 132.82(11) . .
N4 Ho1 N3 88.87(11) . .
N2 Ho1 N3 65.25(11) . .
O1W Ho1 N5 139.14(10) . .
O1W Ho1 N5 74.24(10) 3_666 .
N6 Ho1 N5 68.60(11) . .
N1 Ho1 N5 129.63(11) . .
N4 Ho1 N5 67.10(11) . .
N2 Ho1 N5 131.11(10) . .
N3 Ho1 N5 80.17(11) . .
O1W Ho1 Ho1 33.95(7) . 3_666
O1W Ho1 Ho1 33.41(7) 3_666 3_666
N6 Ho1 Ho1 89.83(8) . 3_666
N1 Ho1 Ho1 107.64(7) . 3_666
N4 Ho1 Ho1 173.17(8) . 3_666
N2 Ho1 Ho1 108.43(7) . 3_666
N3 Ho1 Ho1 92.83(8) . 3_666
N5 Ho1 Ho1 106.67(7) . 3_666
Se3 Sn1 Se1 111.841(17) . .
Se3 Sn1 Se2 118.951(17) . 3_657
Se1 Sn1 Se2 109.467(16) . 3_657
Se3 Sn1 Se2 111.995(17) . .
Se1 Sn1 Se2 110.054(17) . .
Se2 Sn1 Se2 92.990(15) 3_657 .
Sn1 Se2 Sn1 87.010(15) 3_657 .
Ho1 O1W Ho1 112.64(11) . 3_666
Ho1 O1W H1W 121(3) . .
Ho1 O1W H1W 122(3) 3_666 .
C1 N1 Ho1 114.5(2) . .
C1 N1 H1A 108.6 . .
Ho1 N1 H1A 108.6 . .
C1 N1 H1B 108.6 . .
Ho1 N1 H1B 108.6 . .
H1A N1 H1B 107.6 . .
C3 N2 C2 111.9(3) . .
C3 N2 Ho1 106.0(2) . .
C2 N2 Ho1 111.4(2) . .
C3 N2 H2C 109.2 . .
C2 N2 H2C 109.2 . .
Ho1 N2 H2C 109.2 . .
C4 N3 Ho1 116.6(2) . .
C4 N3 H3A 108.1 . .
Ho1 N3 H3A 108.1 . .
C4 N3 H3B 108.1 . .
Ho1 N3 H3B 108.1 . .
H3A N3 H3B 107.3 . .
C5 N4 Ho1 115.8(2) . .
C5 N4 H4A 108.3 . .
Ho1 N4 H4A 108.3 . .
C5 N4 H4B 108.3 . .
Ho1 N4 H4B 108.3 . .
H4A N4 H4B 107.4 . .
C6 N5 C7 114.9(3) . .
C6 N5 Ho1 114.3(2) . .
C7 N5 Ho1 108.5(2) . .
C6 N5 H5C 106.2 . .
C7 N5 H5C 106.2 . .
Ho1 N5 H5C 106.2 . .
C8 N6 Ho1 117.3(2) . .
C8 N6 H6A 108.0 . .
Ho1 N6 H6A 108.0 . .
C8 N6 H6B 108.0 . .
Ho1 N6 H6B 108.0 . .
H6A N6 H6B 107.2 . .
N1 C1 C2 110.7(3) . .
N1 C1 H1C 109.5 . .
C2 C1 H1C 109.5 . .
N1 C1 H1D 109.5 . .
C2 C1 H1D 109.5 . .
H1C C1 H1D 108.1 . .
N2 C2 C1 109.1(3) . .
N2 C2 H2A 109.9 . .
C1 C2 H2A 109.9 . .
N2 C2 H2B 109.9 . .
C1 C2 H2B 109.9 . .
H2A C2 H2B 108.3 . .
N2 C3 C4 109.6(3) . .
N2 C3 H3C 109.8 . .
C4 C3 H3C 109.8 . .
N2 C3 H3D 109.8 . .
C4 C3 H3D 109.8 . .
H3C C3 H3D 108.2 . .
N3 C4 C3 110.6(3) . .
N3 C4 H4C 109.5 . .
C3 C4 H4C 109.5 . .
N3 C4 H4D 109.5 . .
C3 C4 H4D 109.5 . .
H4C C4 H4D 108.1 . .
N4 C5 C6 108.8(3) . .
N4 C5 H5A 109.9 . .
C6 C5 H5A 109.9 . .
N4 C5 H5B 109.9 . .
C6 C5 H5B 109.9 . .
H5A C5 H5B 108.3 . .
N5 C6 C5 112.0(3) . .
N5 C6 H6C 109.2 . .
C5 C6 H6C 109.2 . .
N5 C6 H6D 109.2 . .
C5 C6 H6D 109.2 . .
H6C C6 H6D 107.9 . .
N5 C7 C8 112.4(3) . .
N5 C7 H7A 109.1 . .
C8 C7 H7A 109.1 . .
N5 C7 H7B 109.1 . .
C8 C7 H7B 109.1 . .
H7A C7 H7B 107.9 . .
N6 C8 C7 111.3(3) . .
N6 C8 H8A 109.4 . .
C7 C8 H8A 109.4 . .
N6 C8 H8B 109.4 . .
C7 C8 H8B 109.4 . .
H8A C8 H8B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho1 O1W 2.231(3) .
Ho1 O1W 2.263(3) 3_666
Ho1 N6 2.497(3) .
Ho1 N1 2.529(3) .
Ho1 N4 2.537(3) .
Ho1 N2 2.545(3) .
Ho1 N3 2.547(3) .
Ho1 N5 2.584(3) .
Ho1 Ho1 3.7393(4) 3_666
Sn1 Se3 2.4560(5) .
Sn1 Se1 2.4685(5) .
Sn1 Se2 2.5754(5) 3_657
Sn1 Se2 2.6092(5) .
Se2 Sn1 2.5754(5) 3_657
O1W Ho1 2.263(3) 3_666
O1W H1W 0.831(19) .
N1 C1 1.476(5) .
N1 H1A 0.9000 .
N1 H1B 0.9000 .
N2 C3 1.474(5) .
N2 C2 1.479(5) .
N2 H2C 0.9100 .
N3 C4 1.486(5) .
N3 H3A 0.9000 .
N3 H3B 0.9000 .
N4 C5 1.473(5) .
N4 H4A 0.9000 .
N4 H4B 0.9000 .
N5 C6 1.480(5) .
N5 C7 1.481(5) .
N5 H5C 0.9100 .
N6 C8 1.483(5) .
N6 H6A 0.9000 .
N6 H6B 0.9000 .
C1 C2 1.497(5) .
C1 H1C 0.9700 .
C1 H1D 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.515(6) .
C3 H3C 0.9700 .
C3 H3D 0.9700 .
C4 H4C 0.9700 .
C4 H4D 0.9700 .
C5 C6 1.521(6) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 H6C 0.9700 .
C6 H6D 0.9700 .
C7 C8 1.510(6) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
