#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:37:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179069 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/31/4303157.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_4303157
loop_
_publ_author_name
'Di-Chang Zhong'
'Jian-Bin Lin'
'Wen-Guan Lu'
'Long Jiang'
'Tong-Bu Lu'
_publ_section_title
;
Strong Hydrogen Binding within a 3D Microporous Metal-Organic Framework
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8656
_journal_page_last               8658
_journal_paper_doi               10.1021/ic900968d
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C9 H25 Cd5 N37 O11'
_chemical_formula_weight         1389.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   13.0732(10)
_cell_length_b                   13.0732(10)
_cell_length_c                   13.435(2)
_cell_measurement_reflns_used    2751
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.35
_cell_volume                     1988.5(4)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0893
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6259
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.726
_exptl_absorpt_correction_T_max  0.5490
_exptl_absorpt_correction_T_min  0.4403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (SHELDRICK, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.708
_refine_diff_density_min         -3.057
_refine_diff_density_rms         0.345
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         700
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0761
_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)+(0.1699P)²+22.8956P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2145
_refine_ls_wR_factor_ref         0.2255
_reflns_number_gt                566
_reflns_number_total             700
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900968d_si_002.cif
_cod_data_source_block           l811013m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1988.6(4)
_cod_database_code               4303157
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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
Cd1 Cd 0.5000 0.5000 0.5000 0.0101(6) Uani 1 4 d S . .
Cd2 Cd 0.3333 0.6667 0.40339(12) 0.0176(7) Uani 1 6 d S . .
N1 N 0.5021(9) 0.7511(5) 0.5024(7) 0.015(3) Uani 1 2 d S . .
N2 N 0.5582(7) 0.6964(7) 0.5344(6) 0.0163(17) Uani 1 1 d . . .
N3 N 0.4174(4) 0.8348(9) 0.2995(7) 0.015(2) Uani 1 2 d S . .
N4 N 0.4735(5) 0.9469(10) 0.3313(8) 0.017(3) Uani 1 2 d S . .
N5 N 0.6512(8) 0.7747(9) 0.5862(7) 0.022(2) Uani 0.50 1 d P . .
N6 N 0.6667 0.3333 0.2500 0.044(5) Uani 1 12 d SDU . .
C1 C 0.5066(9) 1.0131(18) 0.2500 0.023(6) Uani 1 4 d S . .
H1 H 0.5485 1.0968 0.2500 0.028 Uiso 1 4 d SR . .
C2 C 0.6512(8) 0.7747(9) 0.5862(7) 0.022(2) Uani 0.50 1 d P . .
H2 H 0.7088 0.7615 0.6184 0.027 Uiso 0.50 1 d PR . .
O1 O 0.7215(4) 0.4431(9) 0.2500 0.138(7) Uani 1 4 d SDU . .
O1W O 0.0000 0.0000 0.6017(18) 0.056(7) Uani 1 6 d S . .
O2W O 0.8808(7) 0.7617(14) 0.6477(11) 0.066(4) Uani 1 2 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0131(8) 0.0131(8) 0.0065(10) 0.0002(2) -0.0002(2) 0.0083(6)
Cd2 0.0176(8) 0.0176(8) 0.0177(10) 0.000 0.000 0.0088(4)
N1 0.014(7) 0.013(5) 0.018(7) -0.002(2) -0.004(4) 0.007(3)
N2 0.018(4) 0.019(5) 0.016(4) 0.000(3) 0.000(3) 0.013(4)
N3 0.019(4) 0.014(6) 0.009(5) 0.004(5) 0.002(2) 0.007(3)
N4 0.027(5) 0.014(6) 0.006(5) -0.004(5) -0.002(2) 0.007(3)
N5 0.018(5) 0.023(5) 0.027(5) -0.007(4) -0.014(4) 0.011(4)
N6 0.043(5) 0.043(5) 0.047(8) 0.000 0.000 0.021(3)
C1 0.040(12) 0.009(10) 0.011(12) 0.000 0.000 0.005(5)
C2 0.018(5) 0.023(5) 0.027(5) -0.007(4) -0.014(4) 0.011(4)
O1 0.137(8) 0.138(7) 0.140(9) 0.000 0.000 0.069(4)
O1W 0.071(12) 0.071(12) 0.028(12) 0.000 0.000 0.035(6)
O2W 0.082(9) 0.077(11) 0.039(7) -0.008(8) -0.004(4) 0.039(5)
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'
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
_geom_angle_publ_flag
N2 Cd1 N2 180.000(1) 13_666 . ?
N2 Cd1 N2 88.8(4) 13_666 19_665 ?
N2 Cd1 N2 91.2(4) . 19_665 ?
N2 Cd1 N2 91.2(4) 13_666 7_556 ?
N2 Cd1 N2 88.8(4) . 7_556 ?
N2 Cd1 N2 180.000(1) 19_665 7_556 ?
N2 Cd1 N4 91.1(3) 13_666 15_656 ?
N2 Cd1 N4 88.9(3) . 15_656 ?
N2 Cd1 N4 88.9(3) 19_665 15_656 ?
N2 Cd1 N4 91.1(3) 7_556 15_656 ?
N2 Cd1 N4 88.9(3) 13_666 3_565 ?
N2 Cd1 N4 91.1(3) . 3_565 ?
N2 Cd1 N4 91.1(3) 19_665 3_565 ?
N2 Cd1 N4 88.9(3) 7_556 3_565 ?
N4 Cd1 N4 180.0 15_656 3_565 ?
N1 Cd2 N1 90.6(4) 2_665 . ?
N1 Cd2 N1 90.6(4) 2_665 3_565 ?
N1 Cd2 N1 90.6(4) . 3_565 ?
N1 Cd2 N3 90.4(3) 2_665 2_665 ?
N1 Cd2 N3 178.6(4) . 2_665 ?
N1 Cd2 N3 90.4(3) 3_565 2_665 ?
N1 Cd2 N3 90.4(3) 2_665 . ?
N1 Cd2 N3 90.4(3) . . ?
N1 Cd2 N3 178.6(4) 3_565 . ?
N3 Cd2 N3 88.6(4) 2_665 . ?
N1 Cd2 N3 178.6(4) 2_665 3_565 ?
N1 Cd2 N3 90.4(3) . 3_565 ?
N1 Cd2 N3 90.4(3) 3_565 3_565 ?
N3 Cd2 N3 88.6(4) 2_665 3_565 ?
N3 Cd2 N3 88.6(4) . 3_565 ?
N2 N1 N2 109.3(10) 21_565 . ?
N2 N1 Cd2 125.3(5) 21_565 . ?
N2 N1 Cd2 125.3(5) . . ?
N1 N2 N5 107.1(8) . . ?
N1 N2 Cd1 124.5(6) . . ?
N5 N2 Cd1 128.4(6) . . ?
N3 N3 N4 108.6(6) 16_556 . ?
N3 N3 Cd2 126.3(3) 16_556 . ?
N4 N3 Cd2 125.1(8) . . ?
C1 N4 N3 105.8(11) . . ?
C1 N4 Cd1 130.7(10) . 2_665 ?
N3 N4 Cd1 123.5(8) . 2_665 ?
N2 N5 C2 108.2(5) . 21_565 ?
N2 N5 N5 108.2(5) . 21_565 ?
C2 N5 N5 0.0(11) 21_565 21_565 ?
N2 N5 H2 126.8 . . ?
C2 N5 H2 125.0 21_565 . ?
N5 N5 H2 125.0 21_565 . ?
O1 N6 O1 120.000(2) 3_665 . ?
O1 N6 O1 120.000(1) 3_665 2_655 ?
O1 N6 O1 120.000(2) . 2_655 ?
N4 C1 N4 111.1(18) 16_556 . ?
N4 C1 H1 124.5 16_556 . ?
N4 C1 H1 124.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N2 2.331(8) 13_666 ?
Cd1 N2 2.331(8) . ?
Cd1 N2 2.331(8) 19_665 ?
Cd1 N2 2.331(8) 7_556 ?
Cd1 N4 2.345(11) 15_656 ?
Cd1 N4 2.345(11) 3_565 ?
Cd2 N1 2.329(10) 2_665 ?
Cd2 N1 2.329(10) . ?
Cd2 N1 2.329(10) 3_565 ?
Cd2 N3 2.361(10) 2_665 ?
Cd2 N3 2.361(10) . ?
Cd2 N3 2.361(10) 3_565 ?
N1 N2 1.325(10) 21_565 ?
N1 N2 1.325(10) . ?
N2 N5 1.328(12) . ?
N3 N3 1.33(2) 16_556 ?
N3 N4 1.339(16) . ?
N4 C1 1.324(16) . ?
N4 Cd1 2.345(11) 2_665 ?
N5 C2 1.33(2) 21_565 ?
N5 N5 1.33(2) 21_565 ?
N5 H2 0.9567 . ?
N6 O1 1.242(10) 3_665 ?
N6 O1 1.242(10) . ?
N6 O1 1.242(10) 2_655 ?
C1 N4 1.324(16) 16_556 ?
C1 H1 0.9477 . ?
