#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:05:36 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179612 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/76/4507617.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_4507617
loop_
_publ_author_name
'Hou, Juan-Juan'
'Zhang, Rong'
'Qin, Ying-Lian'
'Zhang, Xian-Ming'
_publ_section_title
;
 From (3,6)-Connectedkgd,chiralanhto (3,8)-connectedtfz-dNets in Low
 Nuclear Metal Cluster-Based Networks with Triangular
 Pyridinedicarboxylate Ligand
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1618
_journal_paper_doi               10.1021/cg301827p
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C29 H27 N3 Ni2 O12.5'
_chemical_formula_weight         734.9
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.7647(2)
_cell_length_b                   10.7647(2)
_cell_length_c                   26.7578(10)
_cell_measurement_temperature    298(2)
_cell_volume                     2685.25(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4240
_diffrn_reflns_theta_full        28.73
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  0.8436
_exptl_absorpt_correction_T_min  0.7705
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             999
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
;
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.134(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0509P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0763
_reflns_number_gt                4056
_reflns_number_total             4240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301827p_si_001.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P3(2)21
_cod_database_code               4507617
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'
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
Ni1 Ni 0.78123(2) 0.83231(2) 0.133321(7) 0.02477(8) Uani 1 1 d .
N1 N 0.89842(17) 0.32052(18) 0.22781(5) 0.0293(3) Uani 1 1 d .
O1 O 0.9473(2) 0.63446(18) 0.12747(6) 0.0504(4) Uani 1 1 d .
O2 O 0.80314(15) 0.68326(14) 0.17337(4) 0.0306(3) Uani 1 1 d .
O3 O 0.20424(15) 0.22098(17) 0.42289(5) 0.0355(3) Uani 1 1 d .
O4 O 0.33841(15) 0.17265(16) 0.47454(5) 0.0336(3) Uani 1 1 d .
O1W O 0.89365(19) 0.80612(19) 0.07396(5) 0.0471(4) Uani 1 1 d .
O2W O 0.97629(18) 1.0000 0.1667 0.0363(4) Uani 1 2 d S
C1 C 0.9188(2) 0.4276(2) 0.19691(6) 0.0295(4) Uani 1 1 d .
H1A H 0.9850 0.4522 0.1711 0.035 Uiso 1 1 calc R
C2 C 0.8469(2) 0.5026(2) 0.20140(6) 0.0289(4) Uani 1 1 d .
C3 C 0.7479(2) 0.4656(2) 0.23977(7) 0.0344(4) Uani 1 1 d .
H3A H 0.6956 0.5126 0.2430 0.041 Uiso 1 1 calc R
C4 C 0.7268(2) 0.3587(2) 0.27333(7) 0.0345(4) Uani 1 1 d .
C5 C 0.8060(2) 0.2902(2) 0.26581(7) 0.0329(4) Uani 1 1 d .
H5A H 0.7942 0.2194 0.2884 0.039 Uiso 1 1 calc R
C6 C 0.6201(2) 0.3151(2) 0.31468(7) 0.0368(4) Uani 1 1 d .
C7 C 0.4950(3) 0.3221(3) 0.30719(8) 0.0443(6) Uani 1 1 d .
H7A H 0.4786 0.3515 0.2764 0.053 Uiso 1 1 calc R
C8 C 0.3960(2) 0.2858(3) 0.34492(7) 0.0393(5) Uani 1 1 d .
H8A H 0.3132 0.2904 0.3391 0.047 Uiso 1 1 calc R
C9 C 0.4170(2) 0.2426(2) 0.39137(7) 0.0330(4) Uani 1 1 d .
C10 C 0.5395(2) 0.2314(3) 0.39848(7) 0.0413(5) Uani 1 1 d .
H10A H 0.5540 0.1992 0.4290 0.050 Uiso 1 1 calc R
C11 C 0.6402(2) 0.2679(3) 0.36055(7) 0.0432(5) Uani 1 1 d .
H11A H 0.7216 0.2606 0.3660 0.052 Uiso 1 1 calc R
C12 C 0.8692(2) 0.6182(2) 0.16397(7) 0.0298(4) Uani 1 1 d .
C13 C 0.3110(2) 0.20907(19) 0.43302(6) 0.0281(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'
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
O3 Ni1 O2 173.66(6) 2_664 .
O3 Ni1 O4 100.27(6) 2_664 6_665
O2 Ni1 O4 85.68(5) . 6_665
O3 Ni1 O1W 84.75(6) 2_664 .
O2 Ni1 O1W 89.47(6) . .
O4 Ni1 O1W 173.76(6) 6_665 .
O3 Ni1 N1 89.89(6) 2_664 5_565
O2 Ni1 N1 93.14(6) . 5_565
O4 Ni1 N1 82.28(6) 6_665 5_565
O1W Ni1 N1 94.10(7) . 5_565
O3 Ni1 O2W 87.98(5) 2_664 .
O2 Ni1 O2W 89.65(5) . .
O4 Ni1 O2W 91.59(5) 6_665 .
O1W Ni1 O2W 92.29(6) . .
N1 Ni1 O2W 173.05(6) 5_565 .
C5 N1 C1 117.24(16) . .
C5 N1 Ni1 121.69(13) . 5_665
C1 N1 Ni1 117.16(11) . 5_665
C12 O2 Ni1 131.17(11) . .
C13 O3 Ni1 131.55(12) . 3_565
C13 O4 Ni1 135.09(13) . 6_655
Ni1 O2W Ni1 112.74(9) 5_675 .
N1 C1 C2 123.45(16) . .
C1 C2 C3 118.25(16) . .
C1 C2 C12 121.23(16) . .
C3 C2 C12 120.45(17) . .
C4 C3 C2 120.11(18) . .
C3 C4 C5 117.15(17) . .
C3 C4 C6 121.55(18) . .
C5 C4 C6 121.27(17) . .
N1 C5 C4 123.72(17) . .
C11 C6 C7 118.48(18) . .
C11 C6 C4 122.41(18) . .
C7 C6 C4 119.12(17) . .
C8 C7 C6 120.61(19) . .
C7 C8 C9 121.4(2) . .
C8 C9 C10 118.12(17) . .
C8 C9 C13 120.93(18) . .
C10 C9 C13 120.95(17) . .
C11 C10 C9 120.84(18) . .
C6 C11 C10 120.51(19) . .
O1 C12 O2 127.93(17) . .
O1 C12 C2 116.85(17) . .
O2 C12 C2 115.19(15) . .
O3 C13 O4 126.40(16) . .
O3 C13 C9 116.19(16) . .
O4 C13 C9 117.40(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O3 2.0127(13) 2_664
Ni1 O2 2.0389(12) .
Ni1 O4 2.0400(13) 6_665
Ni1 O1W 2.0997(14) .
Ni1 N1 2.1094(16) 5_565
Ni1 O2W 2.1618(11) .
N1 C5 1.344(2) .
N1 C1 1.344(2) .
N1 Ni1 2.1094(16) 5_665
O1 C12 1.243(2) .
O2 C12 1.248(2) .
O3 C13 1.248(2) .
O3 Ni1 2.0127(13) 3_565
O4 C13 1.261(2) .
O4 Ni1 2.0400(13) 6_655
O2W Ni1 2.1618(11) 5_675
C1 C2 1.375(3) .
C2 C3 1.387(3) .
C2 C12 1.520(2) .
C3 C4 1.386(3) .
C4 C5 1.394(3) .
C4 C6 1.491(2) .
C6 C11 1.386(3) .
C6 C7 1.401(3) .
C7 C8 1.375(3) .
C8 C9 1.385(3) .
C9 C10 1.396(3) .
C9 C13 1.504(2) .
C10 C11 1.390(3) .
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
_platon_squeeze_void_content
1 0.000 0.000 -0.011 994 241 ' '
