#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:48:18 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180449 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/18/7211831.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_7211831
loop_
_publ_author_name
'Meng, Qing-Guo'
'Yan, Si-Tang'
'Kong, Guo-Qiang'
'Yang, Xiu-Li'
'Wu, Chuan-De'
_publ_section_title
;
 Formation of a 2D supramolecular water framework via metal--organic unit
 templating
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              688
_journal_paper_doi               10.1039/b915253a
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C39 H61 N5 Ni2 O24'
_chemical_formula_weight         1101.35
_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                110.270(7)
_cell_angle_beta                 107.369(7)
_cell_angle_gamma                100.928(5)
_cell_formula_units_Z            1
_cell_length_a                   10.2608(8)
_cell_length_b                   11.4119(8)
_cell_length_c                   13.314(2)
_cell_measurement_reflns_used    20611
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.72
_cell_measurement_theta_min      1.78
_cell_volume                     1318.9(3)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens XPREP'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0795
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20611
_diffrn_reflns_theta_full        27.72
_diffrn_reflns_theta_max         27.72
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Bloc
_exptl_crystal_F_000             578
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0481
_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)+(0.0532P)²+0.0279P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                3837
_reflns_number_total             6096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b915253a.txt
_cod_data_source_block           Ni
_cod_original_cell_volume        1318.9(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7211831
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
Ni1 Ni 0.17292(4) 0.30374(4) 0.36729(3) 0.03182(13) Uani 1 1 d .
O1 O 0.3931(2) 0.1690(2) 0.26437(16) 0.0414(5) Uani 1 1 d .
O2 O 0.30275(18) 0.19433(18) 0.40055(14) 0.0297(4) Uani 1 1 d .
O3 O 0.5284(2) 0.40088(18) 0.65309(15) 0.0355(5) Uani 1 1 d .
O4 O 0.6218(2) 0.32707(19) 0.52224(17) 0.0391(5) Uani 1 1 d .
O5 O 0.0645(2) 0.4383(2) 0.3442(2) 0.0637(7) Uani 1 1 d .
H5B H -0.0364 0.4202 0.3173 0.096 Uiso 1 1 d .
H5C H 0.0871 0.4636 0.4067 0.096 Uiso 1 1 d .
O6 O 0.3199(2) 0.46777(19) 0.52022(15) 0.0348(5) Uani 1 1 d .
H6A H 0.3979 0.4581 0.5641 0.052 Uiso 1 1 d .
H6B H 0.3642 0.5288 0.4925 0.052 Uiso 1 1 d .
O7 O 0.27235(19) 0.35475(18) 0.26650(15) 0.0334(5) Uani 1 1 d .
H7A H 0.3262 0.2978 0.2621 0.050 Uiso 1 1 d .
H7B H 0.3493 0.4334 0.2981 0.050 Uiso 1 1 d .
O101 O 0.3864(3) 0.3321(3) 0.9530(3) 0.0949(10) Uani 1 1 d .
H10D H 0.4490 0.3844 1.0212 0.142 Uiso 1 1 d .
H10E H 0.4012 0.3662 0.9073 0.142 Uiso 1 1 d .
O102 O 0.4937(3) -0.1319(3) 0.0468(2) 0.0858(9) Uani 1 1 d .
H10J H 0.5408 -0.1835 0.0539 0.129 Uiso 1 1 d .
H10K H 0.5526 -0.0583 0.0794 0.129 Uiso 1 1 d .
O103 O 0.6089(3) 0.1576(3) 0.1834(2) 0.0681(7) Uani 1 1 d .
H10H H 0.5224 0.1745 0.1908 0.102 Uiso 1 1 d .
H10I H 0.5608 0.1586 0.1122 0.102 Uiso 1 1 d .
O104 O 0.4178(3) 0.4748(3) 0.8223(2) 0.0765(8) Uani 1 1 d .
H10F H 0.4539 0.4458 0.7753 0.115 Uiso 1 1 d .
H10G H 0.3652 0.5119 0.7934 0.115 Uiso 1 1 d .
O105 O -0.2177(2) 0.4255(2) 0.30242(19) 0.0596(7) Uani 1 1 d .
H10B H -0.2404 0.4525 0.3583 0.089 Uiso 1 1 d .
H10C H -0.2716 0.3407 0.2597 0.089 Uiso 1 1 d .
N1 N 0.0684(3) 0.2456(2) 0.4637(2) 0.0390(6) Uani 1 1 d .
N2 N 0.0218(3) 0.1434(3) 0.2157(2) 0.0435(6) Uani 1 1 d .
N3 N 0.0382(9) 0.4899(7) 0.1108(7) 0.169(3) Uani 0.50 1 d P
C20 C 0.0382(9) 0.4899(7) 0.1108(7) 0.169(3) Uani 0.50 1 d P
H20A H 0.0612 0.4817 0.1806 0.203 Uiso 0.50 1 calc PR
C1 C 0.5611(3) 0.3109(3) 0.5869(2) 0.0302(6) Uani 1 1 d .
C2 C 0.5344(3) 0.1796(3) 0.5924(2) 0.0271(6) Uani 1 1 d .
C3 C 0.5750(3) 0.1815(3) 0.7010(2) 0.0364(7) Uani 1 1 d .
H3A H 0.5922 0.2585 0.7652 0.044 Uiso 1 1 calc R
C4 C 0.4921(3) 0.0575(2) 0.4919(2) 0.0239(6) Uani 1 1 d .
C5 C 0.4093(3) -0.0693(3) 0.2839(2) 0.0373(7) Uani 1 1 d .
H5A H 0.3821 -0.0728 0.2094 0.045 Uiso 1 1 calc R
C6 C 0.4329(3) 0.0456(3) 0.3755(2) 0.0273(6) Uani 1 1 d .
C7 C 0.3756(3) 0.1466(3) 0.3459(2) 0.0296(6) Uani 1 1 d .
C8 C 0.1398(4) 0.2293(3) 0.5566(3) 0.0512(9) Uani 1 1 d .
H8A H 0.2389 0.2456 0.5794 0.061 Uiso 1 1 calc R
C9 C 0.0730(5) 0.1894(5) 0.6201(4) 0.0784(13) Uani 1 1 d .
H9A H 0.1265 0.1804 0.6854 0.094 Uiso 1 1 calc R
C10 C -0.0729(5) 0.1631(5) 0.5863(4) 0.0900(15) Uani 1 1 d .
H10A H -0.1200 0.1365 0.6284 0.108 Uiso 1 1 calc R
C11 C -0.1485(4) 0.1766(5) 0.4895(4) 0.0819(14) Uani 1 1 d .
H11A H -0.2482 0.1573 0.4635 0.098 Uiso 1 1 calc R
C12 C -0.0739(4) 0.2191(4) 0.4318(4) 0.0653(11) Uani 1 1 d .
H12A H -0.1253 0.2300 0.3670 0.078 Uiso 1 1 calc R
C13 C -0.0580(4) 0.1564(5) 0.1235(3) 0.0656(11) Uani 1 1 d .
H13A H -0.0457 0.2404 0.1259 0.079 Uiso 1 1 calc R
C14 C -0.1602(5) 0.0468(6) 0.0228(3) 0.0866(16) Uani 1 1 d .
H14A H -0.2146 0.0576 -0.0411 0.104 Uiso 1 1 calc R
C15 C -0.1786(5) -0.0746(6) 0.0200(4) 0.0917(17) Uani 1 1 d .
H15A H -0.2473 -0.1482 -0.0455 0.110 Uiso 1 1 calc R
C16 C -0.0964(5) -0.0892(4) 0.1132(3) 0.0811(13) Uani 1 1 d .
H16A H -0.1070 -0.1724 0.1121 0.097 Uiso 1 1 calc R
C17 C 0.0020(4) 0.0216(4) 0.2085(3) 0.0576(10) Uani 1 1 d .
H17A H 0.0585 0.0112 0.2719 0.069 Uiso 1 1 calc R
C18 C -0.0814(11) 0.5194(9) 0.0610(10) 0.185(4) Uani 1 1 d .
H18A H -0.1376 0.5344 0.1062 0.222 Uiso 1 1 d .
C19 C 0.1197(9) 0.4739(8) 0.0449(11) 0.178(5) Uani 1 1 d .
H19A H 0.2102 0.4571 0.0672 0.214 Uiso 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
O2 Ni1 O7 91.87(7) . .
O2 Ni1 N2 92.20(9) . .
O7 Ni1 N2 88.20(9) . .
O2 Ni1 N1 87.73(8) . .
O7 Ni1 N1 177.92(9) . .
N2 Ni1 N1 89.77(10) . .
O2 Ni1 O6 89.44(7) . .
O7 Ni1 O6 92.49(7) . .
N2 Ni1 O6 178.20(8) . .
N1 Ni1 O6 89.55(9) . .
O2 Ni1 O5 172.39(9) . .
O7 Ni1 O5 84.48(8) . .
N2 Ni1 O5 94.35(10) . .
N1 Ni1 O5 96.16(9) . .
O6 Ni1 O5 84.07(9) . .
C7 O2 Ni1 129.08(16) . .
Ni1 O5 H5B 125.5 . .
Ni1 O5 H5C 82.8 . .
H5B O5 H5C 103.1 . .
Ni1 O6 H6A 118.4 . .
Ni1 O6 H6B 104.4 . .
H6A O6 H6B 101.1 . .
Ni1 O7 H7A 98.3 . .
Ni1 O7 H7B 121.7 . .
H7A O7 H7B 97.3 . .
H10D O101 H10E 106.5 . .
H10J O102 H10K 106.2 . .
H10H O103 H10I 77.7 . .
H10F O104 H10G 104.6 . .
H10B O105 H10C 106.6 . .
C8 N1 C12 117.3(3) . .
C8 N1 Ni1 121.7(2) . .
C12 N1 Ni1 121.0(2) . .
C17 N2 C13 117.4(3) . .
C17 N2 Ni1 119.8(2) . .
C13 N2 Ni1 122.8(3) . .
C18 N3 C19 111.7(8) . .
O4 C1 O3 124.0(3) . .
O4 C1 C2 117.4(2) . .
O3 C1 C2 118.5(2) . .
C3 C2 C4 119.7(2) . .
C3 C2 C1 117.1(2) . .
C4 C2 C1 122.4(2) . .
C2 C3 C5 120.7(2) . 2_656
C2 C3 H3A 119.6 . .
C5 C3 H3A 119.6 2_656 .
C6 C4 C4 118.6(3) . 2_656
C6 C4 C2 122.4(2) . .
C4 C4 C2 119.0(3) 2_656 .
C6 C5 C3 121.6(2) . 2_656
C6 C5 H5A 119.2 . .
C3 C5 H5A 119.2 2_656 .
C5 C6 C4 119.6(2) . .
C5 C6 C7 116.4(2) . .
C4 C6 C7 123.5(2) . .
O1 C7 O2 125.1(2) . .
O1 C7 C6 118.8(2) . .
O2 C7 C6 115.8(2) . .
N1 C8 C9 122.6(3) . .
N1 C8 H8A 118.7 . .
C9 C8 H8A 118.7 . .
C10 C9 C8 119.2(4) . .
C10 C9 H9A 120.4 . .
C8 C9 H9A 120.4 . .
C9 C10 C11 119.0(4) . .
C9 C10 H10A 120.5 . .
C11 C10 H10A 120.5 . .
C10 C11 C12 118.4(4) . .
C10 C11 H11A 120.8 . .
C12 C11 H11A 120.8 . .
N1 C12 C11 123.4(4) . .
N1 C12 H12A 118.3 . .
C11 C12 H12A 118.3 . .
N2 C13 C14 121.6(4) . .
N2 C13 H13A 119.2 . .
C14 C13 H13A 119.2 . .
C15 C14 C13 119.0(4) . .
C15 C14 H14A 120.5 . .
C13 C14 H14A 120.5 . .
C14 C15 C16 119.9(4) . .
C14 C15 H15A 120.1 . .
C16 C15 H15A 120.1 . .
C15 C16 C17 118.3(5) . .
C15 C16 H16A 120.8 . .
C17 C16 H16A 120.8 . .
N2 C17 C16 123.7(4) . .
N2 C17 H17A 118.1 . .
C16 C17 H17A 118.1 . .
N3 C18 C19 124.5(9) . 2_565
N3 C18 H18A 113.5 . .
C19 C18 H18A 122.0 2_565 .
N3 C19 C18 123.7(8) . 2_565
N3 C19 H19A 124.0 . .
C18 C19 H19A 112.2 2_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.0472(17) .
Ni1 O7 2.0769(19) .
Ni1 N2 2.079(3) .
Ni1 N1 2.092(2) .
Ni1 O6 2.0928(19) .
Ni1 O5 2.112(2) .
O1 C7 1.251(3) .
O2 C7 1.261(3) .
O3 C1 1.275(3) .
O4 C1 1.245(3) .
O5 H5B 0.9429 .
O5 H5C 0.7233 .
O6 H6A 0.8906 .
O6 H6B 0.9931 .
O7 H7A 0.9275 .
O7 H7B 0.9367 .
O101 H10D 0.8510 .
O101 H10E 0.8618 .
O102 H10J 0.8413 .
O102 H10K 0.8112 .
O103 H10H 0.9684 .
O103 H10I 0.9334 .
O104 H10F 0.8252 .
O104 H10G 0.8330 .
O105 H10B 0.8216 .
O105 H10C 0.8907 .
N1 C8 1.331(4) .
N1 C12 1.333(4) .
N2 C17 1.331(4) .
N2 C13 1.332(4) .
N3 C18 1.373(10) .
N3 C19 1.375(12) .
C1 C2 1.503(4) .
C2 C3 1.371(3) .
C2 C4 1.432(3) .
C3 C5 1.395(4) 2_656
C3 H3A 0.9300 .
C4 C6 1.432(3) .
C4 C4 1.432(5) 2_656
C5 C6 1.365(4) .
C5 C3 1.395(4) 2_656
C5 H5A 0.9300 .
C6 C7 1.504(4) .
C8 C9 1.374(5) .
C8 H8A 0.9300 .
C9 C10 1.367(6) .
C9 H9A 0.9300 .
C10 C11 1.367(6) .
C10 H10A 0.9300 .
C11 C12 1.372(5) .
C11 H11A 0.9300 .
C12 H12A 0.9300 .
C13 C14 1.401(6) .
C13 H13A 0.9300 .
C14 C15 1.348(7) .
C14 H14A 0.9300 .
C15 C16 1.360(6) .
C15 H15A 0.9300 .
C16 C17 1.366(5) .
C16 H16A 0.9300 .
C17 H17A 0.9300 .
C18 C19 1.379(13) 2_565
C18 H18A 0.9468 .
C19 C18 1.379(13) 2_565
C19 H19A 0.9641 .
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
O5 H5B O105 0.94 1.83 2.745(3) 164.2 .
O5 H5C O6 0.72 2.40 2.816(3) 118.6 .
O6 H6A O3 0.89 1.88 2.754(2) 165.6 .
O6 H6B O4 0.99 1.71 2.597(3) 147.0 2_666
O7 H7A O1 0.93 1.74 2.646(3) 164.3 .
O7 H7B O3 0.94 1.83 2.751(3) 168.5 2_666
O101 H10D O104 0.85 1.98 2.830(4) 171.9 2_667
O101 H10E O104 0.86 1.96 2.807(4) 166.6 .
O102 H10J O101 0.84 1.96 2.793(4) 168.4 2_656
O102 H10K O103 0.81 2.22 2.949(4) 149.1 .
O103 H10H O1 0.97 1.87 2.742(3) 147.8 .
O103 H10I O102 0.93 1.92 2.815(4) 160.9 2_655
O104 H10F O3 0.83 1.95 2.766(3) 169.2 .
O104 H10G O105 0.83 2.08 2.903(3) 170.6 2_566
O105 H10B O6 0.82 2.04 2.851(3) 169.8 2_566
O105 H10C O103 0.89 1.93 2.814(4) 173.4 1_455
N3 H20A O5 0.93 2.39 3.301(9) 167.4 .
C20 H20A O5 0.93 2.39 3.301(9) 167.4 .
