#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:55:20 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180485 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/54/7215408.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_7215408
loop_
_publ_author_name
'Huang, Sheng-Li'
'Jin, Guo-Xin'
_publ_section_title
;
 Selective CO2 capture by a 3d--4d coordination polymer material with 1D
 channel
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6013
_journal_paper_doi               10.1039/c1ce05474k
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C24 H40 N6 Ni O13 Pd'
_chemical_formula_weight         785.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 96.896(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.610(5)
_cell_length_b                   18.555(4)
_cell_length_c                   8.2379(16)
_cell_measurement_reflns_used    2059
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.73
_cell_volume                     3734.5(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0838
_diffrn_reflns_av_sigmaI/netI    0.1080
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13781
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        5.90
_exptl_absorpt_coefficient_mu    1.047
_exptl_absorpt_correction_T_max  0.9693
_exptl_absorpt_correction_T_min  0.9026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         4507
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0571
_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)+(0.0775P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1545
_reflns_number_gt                2654
_reflns_number_total             4507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05474k.txt
_cod_data_source_block           mo_00911b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3734.6(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7215408
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Pd1 Pd 0.0000 0.0000 0.5000 0.02194(16) Uani 1 2 d S
Ni1 Ni 0.2500 0.2500 0.0000 0.0436(3) Uani 1 2 d S
O1 O 0.03484(14) -0.09017(18) 0.4322(4) 0.0306(8) Uani 1 1 d .
O2 O 0.10165(17) -0.1294(2) 0.2945(5) 0.0484(11) Uani 1 1 d .
O3 O 0.20115(17) 0.1835(2) 0.1384(5) 0.0488(12) Uani 1 1 d .
O4 O 0.2231(2) 0.0674(3) 0.0957(6) 0.0669(14) Uani 1 1 d .
N1 N 0.06018(17) 0.0457(2) 0.3942(5) 0.0246(9) Uani 1 1 d .
N2 N 0.3138(3) 0.2542(6) 0.1849(7) 0.102(3) Uani 1 1 d D
H2' H 0.334(2) 0.2890(12) 0.155(10) 0.11(3) Uiso 1 1 d D
N3 N 0.2903(3) 0.1639(4) -0.0893(9) 0.095(3) Uani 1 1 d D
H3 H 0.2690(16) 0.130(4) -0.057(9) 0.142 Uiso 1 1 d D
C1 C 0.09215(18) -0.0036(3) 0.3289(5) 0.0258(10) Uani 1 1 d .
C2 C 0.1361(2) 0.0184(3) 0.2511(6) 0.0323(13) Uani 1 1 d .
H2 H 0.1589 -0.0164 0.2084 0.039 Uiso 1 1 calc R
C3 C 0.1468(2) 0.0916(3) 0.2352(6) 0.0330(13) Uani 1 1 d .
C4 C 0.1130(2) 0.1396(3) 0.3002(6) 0.0379(14) Uani 1 1 d .
H4 H 0.1195 0.1898 0.2902 0.045 Uiso 1 1 calc R
C5 C 0.0699(2) 0.1171(3) 0.3796(6) 0.0324(12) Uani 1 1 d .
H5 H 0.0471 0.1514 0.4238 0.039 Uiso 1 1 calc R
C6 C 0.0765(2) -0.0803(3) 0.3519(6) 0.0289(12) Uani 1 1 d .
C7 C 0.1945(2) 0.1159(4) 0.1466(7) 0.0430(16) Uani 1 1 d .
C8 C 0.3443(4) 0.1818(6) 0.1628(13) 0.097(3) Uani 1 1 d D
H8A H 0.3823 0.1850 0.2174 0.117 Uiso 1 1 calc R
H8B H 0.3256 0.1420 0.2136 0.117 Uiso 1 1 calc R
C9 C 0.3448(4) 0.1677(6) -0.0093(15) 0.128(5) Uani 1 1 d D
H9A H 0.3650 0.2065 -0.0588 0.154 Uiso 1 1 calc R
H9B H 0.3639 0.1215 -0.0238 0.154 Uiso 1 1 calc R
C10 C 0.2865(5) 0.1554(7) -0.2711(10) 0.115(4) Uani 1 1 d D
H10A H 0.3005 0.1073 -0.2972 0.138 Uiso 1 1 calc R
H10B H 0.3097 0.1922 -0.3159 0.138 Uiso 1 1 calc R
C11 C 0.2278(5) 0.1634(7) -0.3521(12) 0.119(5) Uani 1 1 d .
H11A H 0.2275 0.1511 -0.4691 0.142 Uiso 1 1 calc R
H11B H 0.2054 0.1266 -0.3038 0.142 Uiso 1 1 calc R
C12 C 0.1987(5) 0.2352(9) -0.3437(11) 0.146(6) Uani 1 1 d .
H12A H 0.2225 0.2747 -0.3745 0.175 Uiso 1 1 calc R
H12B H 0.1646 0.2354 -0.4211 0.175 Uiso 1 1 calc R
O5 O 0.2878(4) 0.0207(6) 0.4030(10) 0.132(3) Uani 1 1 d D
H5A H 0.270(5) -0.006(7) 0.465(13) 0.199 Uiso 1 1 d D
H5B H 0.265(4) 0.027(8) 0.317(10) 0.199 Uiso 1 1 d D
O6 O 0.3986(4) 0.9417(6) 0.0240(13) 0.189(4) Uani 1 1 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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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 Pd1 O1 180.0 . 5_556
O1 Pd1 N1 82.38(15) . .
O1 Pd1 N1 97.62(15) 5_556 .
O1 Pd1 N1 97.62(15) . 5_556
O1 Pd1 N1 82.38(15) 5_556 5_556
N1 Pd1 N1 180.0 . 5_556
N2 Ni1 N2 180.0(3) . 7
N2 Ni1 N3 86.3(4) . .
N2 Ni1 N3 93.7(4) 7 .
N2 Ni1 N3 93.7(4) . 7
N2 Ni1 N3 86.3(4) 7 7
N3 Ni1 N3 179.998(1) . 7
N2 Ni1 O3 93.2(2) . .
N2 Ni1 O3 86.8(2) 7 .
N3 Ni1 O3 93.9(2) . .
N3 Ni1 O3 86.1(2) 7 .
N2 Ni1 O3 86.8(2) . 7
N2 Ni1 O3 93.2(2) 7 7
N3 Ni1 O3 86.1(2) . 7
N3 Ni1 O3 93.9(2) 7 7
O3 Ni1 O3 179.998(1) . 7
C6 O1 Pd1 114.7(3) . .
C7 O3 Ni1 133.0(4) . .
C5 N1 C1 120.4(4) . .
C5 N1 Pd1 127.1(4) . .
C1 N1 Pd1 112.5(3) . .
C12 N2 C8 113.2(10) 7 .
C12 N2 Ni1 117.9(7) 7 .
C8 N2 Ni1 102.5(5) . .
C9 N3 C10 114.3(8) . .
C9 N3 Ni1 105.3(7) . .
C10 N3 Ni1 117.6(7) . .
N1 C1 C2 120.5(5) . .
N1 C1 C6 114.9(4) . .
C2 C1 C6 124.6(5) . .
C1 C2 C3 119.9(5) . .
C4 C3 C2 117.8(5) . .
C4 C3 C7 122.2(5) . .
C2 C3 C7 120.0(6) . .
C3 C4 C5 121.8(5) . .
N1 C5 C4 119.6(5) . .
O2 C6 O1 123.9(5) . .
O2 C6 C1 120.5(4) . .
O1 C6 C1 115.5(4) . .
O4 C7 O3 128.0(5) . .
O4 C7 C3 116.5(6) . .
O3 C7 C3 115.5(6) . .
C9 C8 N2 109.4(8) . .
N3 C9 C8 110.2(8) . .
N3 C10 C11 111.8(7) . .
C12 C11 C10 119.5(10) . .
N2 C12 C11 109.0(11) 7 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 O1 1.990(3) .
Pd1 O1 1.990(3) 5_556
Pd1 N1 1.995(4) .
Pd1 N1 1.996(4) 5_556
Ni1 N2 2.053(7) .
Ni1 N2 2.053(7) 7
Ni1 N3 2.062(8) .
Ni1 N3 2.062(8) 7
Ni1 O3 2.144(4) .
Ni1 O3 2.144(4) 7
O1 C6 1.297(6) .
O2 C6 1.227(6) .
O3 C7 1.266(8) .
O4 C7 1.244(8) .
N1 C5 1.353(7) .
N1 C1 1.359(6) .
N2 C12 1.393(12) 7
N2 C8 1.560(13) .
N3 C9 1.423(8) .
N3 C10 1.498(7) .
C1 C2 1.383(7) .
C1 C6 1.494(7) .
C2 C3 1.393(7) .
C3 C4 1.371(8) .
C3 C7 1.523(7) .
C4 C5 1.378(7) .
C8 C9 1.443(13) .
C10 C11 1.524(15) .
C11 C12 1.518(17) .
C12 N2 1.393(12) 7
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
N2 H2' O2 0.87(2) 2.19(4) 2.991(8) 152(8) 4
N3 H3 O4 0.89(2) 2.13(4) 2.978(7) 161(8) .
O5 H5A O4 0.86(2) 2.03(3) 2.888(10) 175(12) 6_556
O5 H5B O4 0.86(2) 2.12(4) 2.956(10) 164(12) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.500 0.000 -0.031 482.3 31.9
2 0.000 0.500 -0.035 482.3 31.9
