#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:33:06 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179066 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/28/4302817.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_4302817
loop_
_publ_author_name
'Miao-Tzu Ding'
'Jing-Yun Wu'
'Yen-Hsiang Liu'
'Kuang-Lieh Lu'
_publ_section_title
;
Dissolution/Reorganization toward the Destruction/Construction of Porous
Cobalt(II)- and Nickel(II)-Carboxylate Coordination Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7457
_journal_page_last               7465
_journal_paper_doi               10.1021/ic900037g
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C20 H46 Na4 Ni2 O37'
_chemical_formula_weight         1087.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.761(4)
_cell_angle_beta                 92.333(4)
_cell_angle_gamma                93.158(4)
_cell_formula_units_Z            1
_cell_length_a                   9.6710(7)
_cell_length_b                   10.2810(7)
_cell_length_c                   11.1449(7)
_cell_measurement_temperature    293(2)
_cell_volume                     1002.22(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '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  0.1196
_diffrn_reflns_av_sigmaI/netI    0.2252
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17141
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.777
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.777
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.0516
_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)+(0.0387P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                1876
_reflns_number_total             4599
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900037g_si_002_4.cif
_cod_data_source_block           cpd8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               4302817
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ni1 Ni 0.72508(6) 0.75103(6) 0.82165(5) 0.02293(18) Uani 1 1 d . . .
Na1 Na 0.43278(19) 0.50368(19) 0.70519(17) 0.0405(5) Uani 1 1 d . . .
Na2 Na 0.77052(18) 1.11478(19) 0.87988(17) 0.0366(5) Uani 1 1 d . . .
O1 O 0.6681(3) 0.8620(3) 0.7161(3) 0.0243(7) Uani 1 1 d . . .
O2 O 0.6302(3) 0.6806(3) 0.5131(3) 0.0357(9) Uani 1 1 d . . .
O3 O 0.3842(3) 0.9570(3) 0.7943(3) 0.0280(8) Uani 1 1 d . . .
O4 O 0.5256(3) 1.1563(3) 0.8645(2) 0.0266(8) Uani 1 1 d . . .
O5 O 0.8258(3) 1.3325(3) 0.6117(3) 0.0481(10) Uani 1 1 d . . .
O6 O 0.8204(4) 1.2595(3) 0.7733(3) 0.0505(10) Uani 1 1 d . . .
O7 O 1.0141(3) 1.0501(3) 0.8486(3) 0.0299(8) Uani 1 1 d . . .
O8 O 1.1421(4) 1.2256(4) 0.8290(3) 0.0528(10) Uani 1 1 d . . .
O9 O 0.7759(3) 0.6370(3) 0.9242(3) 0.0398(9) Uani 1 1 d . . .
H101 H 0.7927 0.6866 1.0052 0.060 Uiso 1 1 d R . .
H102 H 0.8097 0.5595 0.8906 0.060 Uiso 1 1 d R . .
O10 O 0.9280(3) 0.7664(3) 0.7726(3) 0.0319(8) Uani 1 1 d . . .
H103 H 0.9517 0.8504 0.7793 0.048 Uiso 1 1 d R . .
H104 H 0.9234 0.7070 0.6922 0.048 Uiso 1 1 d R . .
O11 O 0.6711(3) 0.5547(3) 0.6701(2) 0.0253(7) Uani 1 1 d . . .
H105 H 0.6611 0.5716 0.6011 0.038 Uiso 1 1 d R . .
H106 H 0.7211 0.4851 0.6564 0.038 Uiso 1 1 d R . .
O12 O 0.5194(3) 0.7574(3) 0.8772(2) 0.0258(8) Uani 1 1 d . . .
H107 H 0.4776 0.8198 0.8563 0.039 Uiso 1 1 d R . .
H108 H 0.5065 0.7801 0.9593 0.039 Uiso 1 1 d R . .
O13 O 0.7713(3) 0.9474(3) 0.9857(2) 0.0257(7) Uani 1 1 d . . .
H109 H 0.7167 0.9790 1.0473 0.039 Uiso 1 1 d R . .
H110 H 0.8478 0.9338 1.0201 0.039 Uiso 1 1 d R . .
O14 O 0.5479(4) 0.4348(3) 0.8661(3) 0.0629(11) Uani 1 1 d . . .
H111 H 0.5383 0.3494 0.8626 0.094 Uiso 1 1 d R . .
H112 H 0.6312 0.4667 0.8880 0.094 Uiso 1 1 d R . .
O15 O 0.2117(3) 0.4286(3) 0.7389(3) 0.0516(10) Uani 1 1 d . . .
H113 H 0.1765 0.3674 0.7682 0.077 Uiso 1 1 d R . .
H114 H 0.1623 0.4095 0.6656 0.077 Uiso 1 1 d R . .
O16 O 0.3032(4) 0.6636(3) 0.6362(3) 0.0593(11) Uani 1 1 d . . .
H115 H 0.3253 0.7538 0.6814 0.089 Uiso 1 1 d R . .
H116 H 0.3488 0.6346 0.5675 0.089 Uiso 1 1 d R . .
O17 O 0.8551(4) 1.2978(4) 1.0833(4) 0.0980(17) Uani 1 1 d . . .
H117 H 0.8179 1.3729 1.1221 0.147 Uiso 1 1 d R . .
H118 H 0.9146 1.2795 1.1316 0.147 Uiso 1 1 d R . .
O18 O 0.0540(4) 0.3794(4) 0.4967(4) 0.0854(14) Uani 1 1 d . . .
H119 H 0.0427 0.4539 0.4874 0.128 Uiso 1 1 d R . .
H120 H -0.0222 0.3553 0.5278 0.128 Uiso 1 1 d R . .
O19 O 0.0000 0.5000 0.0000 0.178(4) Uani 1 2 d S . .
H121 H 0.0260 0.5817 0.0734 0.267 Uiso 0.50 1 d PR . .
H122 H 0.0732 0.4457 -0.0118 0.267 Uiso 0.50 1 d PR . .
C1 C 0.5719(4) 0.8901(4) 0.4178(4) 0.0223(11) Uani 1 1 d . . .
H1 H 0.6212 0.8153 0.3625 0.027 Uiso 1 1 calc R . .
C2 C 0.5581(4) 0.9083(4) 0.5475(4) 0.0195(10) Uani 1 1 d . . .
C3 C 0.4851(4) 1.0204(4) 0.6317(4) 0.0177(10) Uani 1 1 d . . .
C4 C 0.6236(4) 0.8083(5) 0.5950(4) 0.0248(11) Uani 1 1 d . . .
C5 C 0.4631(5) 1.0455(5) 0.7741(4) 0.0237(11) Uani 1 1 d . . .
C6 C 0.9111(4) 1.0615(5) 0.4424(4) 0.0278(11) Uani 1 1 d . . .
H6 H 0.8518 1.1027 0.4030 0.033 Uiso 1 1 calc R . .
C7 C 0.9309(4) 1.1189(5) 0.5801(4) 0.0257(11) Uani 1 1 d . . .
C8 C 1.0203(4) 1.0574(4) 0.6363(4) 0.0232(11) Uani 1 1 d . . .
C9 C 0.8529(5) 1.2471(5) 0.6625(5) 0.0317(12) Uani 1 1 d . . .
C10 C 1.0607(5) 1.1177(5) 0.7836(4) 0.0294(12) 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'
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'
Na Na 0.0362 0.0249 '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
O9 Ni1 O1 178.19(12) . . ?
O9 Ni1 O11 84.48(11) . . ?
O1 Ni1 O11 94.25(11) . . ?
O9 Ni1 O10 92.01(12) . . ?
O1 Ni1 O10 89.39(11) . . ?
O11 Ni1 O10 95.77(11) . . ?
O9 Ni1 O13 92.86(11) . . ?
O1 Ni1 O13 88.34(11) . . ?
O11 Ni1 O13 175.75(11) . . ?
O10 Ni1 O13 87.61(11) . . ?
O9 Ni1 O12 91.69(11) . . ?
O1 Ni1 O12 87.00(11) . . ?
O11 Ni1 O12 88.82(11) . . ?
O10 Ni1 O12 174.37(11) . . ?
O13 Ni1 O12 87.96(10) . . ?
O9 Ni1 Na1 84.05(9) . . ?
O1 Ni1 Na1 94.14(8) . . ?
O11 Ni1 Na1 42.17(8) . . ?
O10 Ni1 Na1 137.92(9) . . ?
O13 Ni1 Na1 134.34(8) . . ?
O12 Ni1 Na1 46.82(8) . . ?
O9 Ni1 Na2 134.93(9) . . ?
O1 Ni1 Na2 46.54(8) . . ?
O11 Ni1 Na2 139.86(8) . . ?
O10 Ni1 Na2 78.44(8) . . ?
O13 Ni1 Na2 43.39(8) . . ?
O12 Ni1 Na2 95.94(8) . . ?
Na1 Ni1 Na2 131.27(4) . . ?
O15 Na1 O2 80.63(12) . 2_666 ?
O15 Na1 O11 173.04(13) . . ?
O2 Na1 O11 97.38(11) 2_666 . ?
O15 Na1 O14 93.68(13) . . ?
O2 Na1 O14 118.01(12) 2_666 . ?
O11 Na1 O14 81.32(12) . . ?
O15 Na1 O16 82.95(13) . . ?
O2 Na1 O16 86.47(11) 2_666 . ?
O11 Na1 O16 103.65(12) . . ?
O14 Na1 O16 154.54(13) . . ?
O15 Na1 O12 113.35(12) . . ?
O2 Na1 O12 155.66(12) 2_666 . ?
O11 Na1 O12 70.93(9) . . ?
O14 Na1 O12 82.15(10) . . ?
O16 Na1 O12 76.18(10) . . ?
O15 Na1 Ni1 149.08(10) . . ?
O2 Na1 Ni1 129.76(10) 2_666 . ?
O11 Na1 Ni1 34.46(6) . . ?
O14 Na1 Ni1 77.59(9) . . ?
O16 Na1 Ni1 92.38(9) . . ?
O12 Na1 Ni1 36.60(6) . . ?
O6 Na2 O17 91.04(15) . . ?
O6 Na2 O4 89.12(12) . . ?
O17 Na2 O4 103.62(13) . . ?
O6 Na2 O13 167.20(14) . . ?
O17 Na2 O13 88.18(13) . . ?
O4 Na2 O13 103.49(11) . . ?
O6 Na2 O7 86.05(12) . . ?
O17 Na2 O7 86.33(13) . . ?
O4 Na2 O7 169.03(12) . . ?
O13 Na2 O7 81.15(11) . . ?
O6 Na2 O1 111.65(12) . . ?
O17 Na2 O1 157.27(14) . . ?
O4 Na2 O1 79.11(10) . . ?
O13 Na2 O1 69.39(9) . . ?
O7 Na2 O1 93.53(11) . . ?
O6 Na2 C10 62.12(13) . . ?
O17 Na2 C10 88.22(15) . . ?
O4 Na2 C10 149.34(13) . . ?
O13 Na2 C10 105.08(12) . . ?
O7 Na2 C10 23.96(10) . . ?
O1 Na2 C10 100.80(12) . . ?
O6 Na2 Ni1 141.46(10) . . ?
O17 Na2 Ni1 123.47(11) . . ?
O4 Na2 Ni1 97.63(9) . . ?
O13 Na2 Ni1 35.66(6) . . ?
O7 Na2 Ni1 80.26(8) . . ?
O1 Na2 Ni1 34.86(6) . . ?
C10 Na2 Ni1 99.06(10) . . ?
C4 O1 Ni1 126.3(3) . . ?
C4 O1 Na2 133.5(3) . . ?
Ni1 O1 Na2 98.61(11) . . ?
C4 O2 Na1 148.0(3) . 2_666 ?
C5 O4 Na2 108.6(3) . . ?
C9 O6 Na2 138.8(3) . . ?
C10 O7 Na2 103.8(3) . . ?
Ni1 O11 Na1 103.37(11) . . ?
Ni1 O12 Na1 96.58(10) . . ?
Ni1 O13 Na2 100.94(10) . . ?
C3 C1 C2 122.2(4) 2_676 . ?
C1 C2 C3 119.6(4) . . ?
C1 C2 C4 119.4(4) . . ?
C3 C2 C4 121.0(4) . . ?
C1 C3 C2 118.2(4) 2_676 . ?
C1 C3 C5 119.1(4) 2_676 . ?
C2 C3 C5 122.7(4) . . ?
O2 C4 O1 125.9(4) . . ?
O2 C4 C2 117.9(4) . . ?
O1 C4 C2 116.2(4) . . ?
O3 C5 O4 124.3(4) . . ?
O3 C5 C3 118.7(4) . . ?
O4 C5 C3 117.0(4) . . ?
C8 C6 C7 120.4(4) 2_776 . ?
C8 C7 C6 118.8(4) . . ?
C8 C7 C9 122.4(4) . . ?
C6 C7 C9 118.8(4) . . ?
C7 C8 C6 120.8(4) . 2_776 ?
C7 C8 C10 123.9(4) . . ?
C6 C8 C10 115.1(4) 2_776 . ?
O6 C9 O5 125.4(4) . . ?
O6 C9 C7 118.0(4) . . ?
O5 C9 C7 116.6(4) . . ?
O8 C10 O7 125.3(4) . . ?
O8 C10 C8 116.1(4) . . ?
O7 C10 C8 118.4(4) . . ?
O8 C10 Na2 122.3(3) . . ?
O7 C10 Na2 52.3(2) . . ?
C8 C10 Na2 98.2(3) . . ?
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
Ni1 O9 2.016(3) . ?
Ni1 O1 2.032(3) . ?
Ni1 O11 2.039(3) . ?
Ni1 O10 2.074(3) . ?
Ni1 O13 2.088(3) . ?
Ni1 O12 2.104(3) . ?
Ni1 Na1 3.5053(19) . ?
Ni1 Na2 3.5160(18) . ?
Na1 O15 2.332(4) . ?
Na1 O2 2.402(3) 2_666 ?
Na1 O11 2.419(3) . ?
Na1 O14 2.438(3) . ?
Na1 O16 2.464(4) . ?
Na1 O12 2.573(3) . ?
Na2 O6 2.303(4) . ?
Na2 O17 2.336(4) . ?
Na2 O4 2.442(3) . ?
Na2 O13 2.460(3) . ?
Na2 O7 2.482(3) . ?
Na2 O1 2.581(3) . ?
Na2 C10 3.048(5) . ?
O1 C4 1.270(5) . ?
O2 C4 1.254(5) . ?
O2 Na1 2.402(3) 2_666 ?
O3 C5 1.253(5) . ?
O4 C5 1.262(5) . ?
O5 C9 1.261(5) . ?
O6 C9 1.242(5) . ?
O7 C10 1.274(5) . ?
O8 C10 1.228(5) . ?
C1 C3 1.382(5) 2_676 ?
C1 C2 1.391(5) . ?
C2 C3 1.394(5) . ?
C2 C4 1.496(6) . ?
C3 C1 1.382(5) 2_676 ?
C3 C5 1.523(5) . ?
C6 C8 1.394(5) 2_776 ?
C6 C7 1.395(5) . ?
C7 C8 1.374(5) . ?
C7 C9 1.517(6) . ?
C8 C6 1.394(5) 2_776 ?
C8 C10 1.517(5) . ?
