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#$Date: 2016-03-21 18:49:09 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178825 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/79/4107914.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_4107914
loop_
_publ_author_name
'Bo Zheng'
'Hao Dong'
'Junfeng Bai'
'Yizhi Li'
'Shuhua Li'
'Manfred Scheer'
_publ_contact_author
;
    Junfeng Bai
    State KeyLab of Coordination Chemistry
    School of Chemistryand Chemical Engineering
    Nanjing University
    Hankou 22, Nanjing 210093
    P.R. China
;
_publ_contact_author_email       bjunfeng@nju.edu.cn
_publ_contact_author_fax         '86 25 83314502'
_publ_contact_author_phone       86-25-83593384
_publ_section_title
;
 Temperature Controlled Reversible Change of the Coordination Modes of the
 Highly Symmetrical Multitopic Ligand To Construct Coordination
 Assemblies: Experimental and Theoretical Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7778
_journal_page_last               7779
_journal_paper_doi               10.1021/ja800439p
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C16 H32 Cd4 O32, 2(H2 O)'
_chemical_formula_sum            'C16 H36 Cd4 O34'
_chemical_formula_weight         1222.05
_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                 99.525(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.9429(9)
_cell_length_b                   16.203(2)
_cell_length_c                   16.022(2)
_cell_measurement_reflns_used    4061
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      28.13
_cell_measurement_theta_min      2.58
_cell_volume                     1777.6(4)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0709
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9455
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    2.479
_exptl_absorpt_correction_T_max  0.598
_exptl_absorpt_correction_T_min  0.497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABA, (Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.283
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.982
_refine_diff_density_min         -2.511
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0508
_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)+(0.08P)²+1.99P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1359
_reflns_number_gt                2909
_reflns_number_total             3475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja800439p-file002.cif
_cod_data_source_block           complex2
_cod_original_cell_volume        1777.5(4)
_cod_original_sg_symbol_H-M      ' P 21/n'
_cod_database_code               4107914
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
C1 C 1.0125(9) 0.1590(4) 0.2740(4) 0.0234(12) Uani 1 1 d .
C2 C 0.9996(9) 0.1759(4) 0.3619(4) 0.0223(12) Uani 1 1 d .
C3 C 1.0065(9) 0.2650(4) 0.3446(4) 0.0222(12) Uani 1 1 d .
C4 C 1.0190(9) 0.2465(4) 0.2562(4) 0.0222(13) Uani 1 1 d .
C5 C 0.9776(9) -0.2469(4) 0.2368(4) 0.0211(12) Uani 1 1 d .
C6 C 0.9984(9) -0.2671(4) 0.1505(4) 0.0241(13) Uani 1 1 d .
C7 C 0.9935(9) -0.3544(4) 0.1703(4) 0.0234(12) Uani 1 1 d .
C8 C 0.9736(9) -0.3339(4) 0.2578(4) 0.0251(13) Uani 1 1 d .
Cd1 Cd 1.00567(7) 0.25907(3) 0.05331(3) 0.02641(17) Uani 1 1 d .
Cd2 Cd 0.97501(7) -0.04417(3) 0.25128(3) 0.02925(18) Uani 1 1 d .
O1 O 1.0184(7) 0.0941(3) 0.2307(3) 0.0320(11) Uani 1 1 d .
O2 O 0.9869(7) 0.1340(3) 0.4261(3) 0.0339(11) Uani 1 1 d .
O3 O 1.0033(8) 0.3287(3) 0.3882(3) 0.0370(12) Uani 1 1 d .
O4 O 1.0309(7) 0.2904(3) 0.1925(3) 0.0294(10) Uani 1 1 d .
O5 O 0.9661(7) -0.1821(3) 0.2783(3) 0.0293(10) Uani 1 1 d .
O6 O 1.0150(7) -0.2251(3) 0.0858(3) 0.0322(11) Uani 1 1 d .
O7 O 1.0066(8) -0.4204(3) 0.1292(3) 0.0357(11) Uani 1 1 d .
O8 O 0.9593(7) -0.3736(3) 0.3225(3) 0.0333(11) Uani 1 1 d .
O9 O 1.2968(8) -0.0534(3) 0.2985(4) 0.0538(16) Uani 1 1 d .
H9A H 1.3178 -0.0485 0.3521 0.081 Uiso 1 1 d R
H9B H 1.3375 -0.1003 0.2849 0.081 Uiso 1 1 d R
O10 O 0.6538(8) -0.0355(3) 0.2019(4) 0.0546(16) Uani 1 1 d .
H10B H 0.6330 0.0049 0.1678 0.082 Uiso 1 1 d R
H10A H 0.6153 -0.0799 0.1761 0.082 Uiso 1 1 d R
O11 O 1.0255(9) -0.0616(3) 0.1134(3) 0.0474(14) Uani 1 1 d .
H11B H 0.9484 -0.0988 0.0900 0.071 Uiso 1 1 d R
H11A H 1.0021 -0.0165 0.0866 0.071 Uiso 1 1 d R
O12 O 0.8974(8) -0.0234(3) 0.3829(3) 0.0421(13) Uani 1 1 d .
H12B H 0.8596 0.0262 0.3868 0.063 Uiso 1 1 d R
H12A H 0.8060 -0.0561 0.3901 0.063 Uiso 1 1 d R
O13 O 1.1266(8) 0.1305(3) 0.0822(3) 0.0417(12) Uani 1 1 d .
H13A H 1.2505 0.1322 0.0885 0.063 Uiso 1 1 d R
H13B H 1.0921 0.1132 0.1276 0.063 Uiso 1 1 d R
O14 O 0.7030(7) 0.1994(3) 0.0489(3) 0.0440(13) Uani 1 1 d .
H14A H 0.7189 0.1416 0.0611 0.066 Uiso 1 1 d R
H14B H 0.6281 0.2066 -0.0066 0.066 Uiso 1 1 d R
O15 O 0.8770(8) 0.3872(3) 0.0216(3) 0.0411(12) Uani 1 1 d .
H15A H 0.9813 0.4257 0.0199 0.062 Uiso 1 1 d R
H15B H 0.7940 0.3857 -0.0326 0.062 Uiso 1 1 d R
O16 O 1.3127(8) 0.3079(4) 0.0570(3) 0.0521(15) Uani 1 1 d .
H16B H 1.3882 0.2857 0.0980 0.078 Uiso 1 1 d R
H16A H 1.3513 0.2959 0.0108 0.078 Uiso 1 1 d R
O1W O 0.2963(10) -0.0091(4) 0.0029(4) 0.074(2) Uani 1 1 d .
H1A H 0.3381 0.0072 0.0530 0.089 Uiso 1 1 d R
H1B H 0.3134 0.0288 -0.0319 0.111 Uiso 1 1 d R
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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 C1 C4 134.5(6) . .
O1 C1 C2 134.6(6) . .
C4 C1 C2 90.8(5) . .
O2 C2 C1 136.1(6) . .
O2 C2 C3 134.2(6) . .
C1 C2 C3 89.7(5) . .
O3 C3 C4 135.9(6) . .
O3 C3 C2 134.7(5) . .
C4 C3 C2 89.4(5) . .
O4 C4 C1 136.1(6) . .
O4 C4 C3 133.8(5) . .
C1 C4 C3 90.0(5) . .
O5 C5 C8 133.4(6) . .
O5 C5 C6 136.0(6) . .
C8 C5 C6 90.6(5) . .
O6 C6 C5 134.3(6) . .
O6 C6 C7 135.6(6) . .
C5 C6 C7 90.1(5) . .
O7 C7 C6 134.6(6) . .
O7 C7 C8 135.5(6) . .
C6 C7 C8 89.9(5) . .
O8 C8 C5 134.9(6) . .
O8 C8 C7 135.6(6) . .
C5 C8 C7 89.4(5) . .
O13 Cd1 O4 92.23(16) . .
O13 Cd1 O16 90.0(2) . .
O4 Cd1 O16 88.68(17) . .
O13 Cd1 O6 86.52(17) . 3_755
O4 Cd1 O6 178.69(16) . 3_755
O16 Cd1 O6 90.93(18) . 3_755
O13 Cd1 O15 178.45(19) . .
O4 Cd1 O15 88.81(17) . .
O16 Cd1 O15 91.1(2) . .
O6 Cd1 O15 92.45(17) 3_755 .
O13 Cd1 O14 85.8(2) . .
O4 Cd1 O14 92.64(17) . .
O16 Cd1 O14 175.6(2) . .
O6 Cd1 O14 87.65(18) 3_755 .
O15 Cd1 O14 93.0(2) . .
O9 Cd2 O10 179.1(2) . .
O9 Cd2 O5 85.83(18) . .
O10 Cd2 O5 94.11(18) . .
O9 Cd2 O12 94.1(2) . .
O10 Cd2 O12 86.8(2) . .
O5 Cd2 O12 87.23(16) . .
O9 Cd2 O1 88.09(18) . .
O10 Cd2 O1 91.99(18) . .
O5 Cd2 O1 173.88(18) . .
O12 Cd2 O1 92.60(16) . .
O9 Cd2 O11 90.8(2) . .
O10 Cd2 O11 88.3(2) . .
O5 Cd2 O11 94.28(17) . .
O12 Cd2 O11 174.9(2) . .
O1 Cd2 O11 86.43(16) . .
C1 O1 Cd2 135.8(4) . .
C4 O4 Cd1 131.9(4) . .
C5 O5 Cd2 135.7(4) . .
C6 O6 Cd1 132.4(4) . 3_755
Cd2 O9 H9A 109.2 . .
Cd2 O9 H9B 109.2 . .
H9A O9 H9B 109.4 . .
Cd2 O10 H10B 109.2 . .
Cd2 O10 H10A 109.4 . .
H10B O10 H10A 109.4 . .
Cd2 O11 H11B 108.9 . .
Cd2 O11 H11A 109.3 . .
H11B O11 H11A 109.5 . .
Cd2 O12 H12B 109.2 . .
Cd2 O12 H12A 109.2 . .
H12B O12 H12A 109.5 . .
Cd1 O13 H13A 109.2 . .
Cd1 O13 H13B 109.4 . .
H13A O13 H13B 109.5 . .
Cd1 O14 H14A 109.3 . .
Cd1 O14 H14B 109.3 . .
H14A O14 H14B 109.5 . .
Cd1 O15 H15A 109.2 . .
Cd1 O15 H15B 109.4 . .
H15A O15 H15B 109.5 . .
Cd1 O16 H16B 109.2 . .
Cd1 O16 H16A 109.2 . .
H16B O16 H16A 109.5 . .
H1A O1W H1B 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.263(7) .
C1 C4 1.449(9) .
C1 C2 1.451(8) .
C2 O2 1.248(7) .
C2 C3 1.471(8) .
C3 O3 1.249(7) .
C3 C4 1.465(8) .
C4 O4 1.258(7) .
C5 O5 1.253(7) .
C5 C8 1.450(8) .
C5 C6 1.451(8) .
C6 O6 1.261(7) .
C6 C7 1.451(9) .
C7 O7 1.268(8) .
C7 C8 1.468(8) .
C8 O8 1.239(7) .
Cd1 O13 2.264(5) .
Cd1 O4 2.265(4) .
Cd1 O16 2.266(5) .
Cd1 O6 2.277(4) 3_755
Cd1 O15 2.283(5) .
Cd1 O14 2.303(5) .
Cd2 O9 2.242(6) .
Cd2 O10 2.244(6) .
Cd2 O5 2.279(4) .
Cd2 O12 2.287(5) .
Cd2 O1 2.292(4) .
Cd2 O11 2.311(5) .
O6 Cd1 2.277(4) 3_755
O9 H9A 0.8505 .
O9 H9B 0.8507 .
O10 H10B 0.8500 .
O10 H10A 0.8499 .
O11 H11B 0.8503 .
O11 H11A 0.8498 .
O12 H12B 0.8502 .
O12 H12A 0.8501 .
O13 H13A 0.8500 .
O13 H13B 0.8502 .
O14 H14A 0.9600 .
O14 H14B 0.9600 .
O15 H15A 0.9600 .
O15 H15B 0.9602 .
O16 H16B 0.8501 .
O16 H16A 0.8496 .
O1W H1A 0.8499 .
O1W H1B 0.8499 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O11 H11A O13 0.85 2.54 3.248(7) 141.6 .
O11 H11B O6 0.85 2.10 2.685(7) 125.3 .
O12 H12B O2 0.85 2.01 2.687(7) 135.9 .
O13 H13B O1 0.85 1.83 2.676(6) 170.3 .
O9 H9B O4 0.85 2.00 2.793(7) 154.9 2_745
O10 H10B O8 0.85 2.08 2.748(7) 134.6 2_655
O10 H10A O3 0.85 1.91 2.755(7) 172.0 2_645
O12 H12A O15 0.85 2.25 3.006(7) 148.6 2_645
O11 H11A O1W 0.85 2.35 2.897(9) 122.3 3_655
O14 H14A O1W 0.96 2.37 3.194(9) 143.1 3_655
O16 H16B O5 0.85 2.14 2.831(7) 138.6 2_755
O13 H13A O8 0.85 2.27 3.024(7) 148.1 2_755
O14 H14B O3 0.96 1.85 2.753(7) 154.8 4_565
O15 H15B O2 0.96 2.15 2.902(7) 134.3 4_565
O16 H16A O2 0.85 2.11 2.754(7) 132.5 4_665
