#------------------------------------------------------------------------------
#$Date: 2019-09-18 20:58:16 +0300 (Wed, 18 Sep 2019) $
#$Revision: 218496 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/09/7200958.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_7200958
loop_
_publ_author_name
'Yao, Qing-Xia'
'Jin, Xu-Hui'
'Ju, Zhan-Feng'
'Zhang, Hai-Xia'
'Zhang, Jie'
_publ_section_title
;
 Supramolecular Borromean sheet consisting of threefold parallel
 interwoven 44-sql layers assembled by a flexible bipyridinium ligand
;
_journal_coden_ASTM              CRECF4
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1502
_journal_page_last               1504
_journal_paper_doi               10.1039/b901516g
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C34 H32 N2 Ni O12, 9(H2O)'
_chemical_formula_sum            'C34 H50 N2 Ni O21'
_chemical_formula_weight         881.46
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 97.012(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.087(4)
_cell_length_b                   23.552(6)
_cell_length_c                   13.954(4)
_cell_measurement_reflns_used    10085
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4642
_cell_measurement_theta_min      3.0315
_cell_volume                     4269(2)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32662
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(R.H. Blessing, 1995&1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lamellate
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.6500
_exptl_crystal_size_mid          0.6500
_exptl_crystal_size_min          0.0700
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         9646
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0750
_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)+(0.1606P)²+1.3480P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2307
_refine_ls_wR_factor_ref         0.2444
_reflns_number_gt                7985
_reflns_number_total             9646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B901516G.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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 

 Replaced the incorrect bibliographical reference to the original
 publication with a proper one.

 Antanas Vaitkus,
 2019-09-18
;
_cod_original_sg_symbol_Hall     -P_2ybc
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7200958
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.58217(3) 0.423141(15) 0.13284(2) 0.03875(17) Uani 1 1 d . . .
O1 O 0.54785(19) 0.41515(10) 0.27108(15) 0.0490(5) Uani 1 1 d . . .
O1W O 0.45188(17) 0.47362(9) 0.09156(14) 0.0432(5) Uani 1 1 d D . .
O2 O 0.41529(18) 0.47397(10) 0.26887(15) 0.0502(5) Uani 1 1 d . . .
O2W O 0.65815(19) 0.49803(10) 0.16850(16) 0.0511(5) Uani 1 1 d D . .
O3 O 0.1882(3) -0.08919(15) 1.1458(2) 0.0831(10) Uani 1 1 d . . .
O3W O 0.7120(2) 0.37629(12) 0.18020(18) 0.0563(6) Uani 1 1 d D . .
O4 O 0.1808(2) -0.00118(15) 1.19901(19) 0.0806(9) Uani 1 1 d . . .
O4W O 0.62605(19) 0.42854(11) -0.00531(17) 0.0482(5) Uani 1 1 d D . .
O5 O 0.48766(17) 0.35417(9) 0.09191(14) 0.0443(5) Uani 1 1 d . . .
O5W O 0.6342(8) 0.2927(4) 0.3039(8) 0.253(5) Uani 1 1 d . . .
O6 O 0.5282(2) 0.33416(12) -0.05575(18) 0.0649(7) Uani 1 1 d . . .
O6W O 0.8574(5) 0.3345(5) 0.0770(6) 0.232(4) Uani 1 1 d . . .
O7 O 0.3321(2) 0.41373(10) -0.04472(18) 0.0563(6) Uani 1 1 d . . .
O7W O 0.9688(7) 0.3980(6) 0.0021(14) 0.381(9) Uani 1 1 d . . .
O8 O 0.1702(3) 0.40211(16) -0.0194(3) 0.1028(12) Uani 1 1 d . . .
O8W O 0.6867(6) 0.2519(4) -0.0243(7) 0.227(4) Uani 1 1 d . . .
O9W O 0.1741(4) 0.5167(2) 0.0396(4) 0.1273(16) Uani 1 1 d . . .
O10W O -0.0127(5) 0.3224(3) 0.6575(7) 0.215(4) Uani 1 1 d . . .
O11W O 0.0818(4) 0.0872(2) 1.2691(4) 0.1248(16) Uani 1 1 d . . .
O12W O 0.0688(5) -0.1792(2) 1.0689(6) 0.179(3) Uani 1 1 d . . .
O13W O 0.6913(12) 0.2361(9) 0.1808(13) 0.422(11) Uani 1 1 d . . .
N1 N 0.4118(2) 0.34849(11) 0.72971(16) 0.0432(5) Uani 1 1 d . . .
N2 N 0.1174(2) 0.09988(13) 0.72704(19) 0.0512(6) Uani 1 1 d . . .
C1 C 0.4807(2) 0.44132(13) 0.31069(19) 0.0400(6) Uani 1 1 d . . .
C2 C 0.4794(2) 0.43078(12) 0.4171(2) 0.0398(6) Uani 1 1 d . . .
C3 C 0.5586(3) 0.40078(14) 0.4699(2) 0.0478(7) Uani 1 1 d . . .
H1 H 0.6134 0.3861 0.4384 0.057 Uiso 1 1 calc R . .
C4 C 0.3993(2) 0.45257(13) 0.4645(2) 0.0424(6) Uani 1 1 d . . .
H2 H 0.3451 0.4736 0.4294 0.051 Uiso 1 1 calc R . .
C5 C 0.5583(3) 0.39210(14) 0.5680(2) 0.0486(7) Uani 1 1 d . . .
H3 H 0.6131 0.3717 0.6035 0.058 Uiso 1 1 calc R . .
C6 C 0.3995(2) 0.44340(14) 0.5625(2) 0.0441(6) Uani 1 1 d . . .
H4 H 0.3451 0.4581 0.5943 0.053 Uiso 1 1 calc R . .
C7 C 0.4786(2) 0.41296(12) 0.6148(2) 0.0416(6) Uani 1 1 d . . .
C8 C 0.4754(3) 0.40087(14) 0.7212(2) 0.0470(7) Uani 1 1 d . . .
H5 H 0.5460 0.3949 0.7540 0.056 Uiso 1 1 calc R . .
H6 H 0.4445 0.4334 0.7521 0.056 Uiso 1 1 calc R . .
C9 C 0.4578(3) 0.29717(15) 0.7341(2) 0.0515(7) Uani 1 1 d . . .
H7 H 0.5307 0.2949 0.7385 0.062 Uiso 1 1 calc R . .
C10 C 0.3091(3) 0.35250(15) 0.7257(2) 0.0530(7) Uani 1 1 d . . .
H8 H 0.2776 0.3889 0.7239 0.064 Uiso 1 1 calc R . .
C11 C 0.4015(3) 0.24871(14) 0.7325(2) 0.0499(7) Uani 1 1 d . . .
H9 H 0.4353 0.2129 0.7355 0.060 Uiso 1 1 calc R . .
C12 C 0.2492(3) 0.30490(15) 0.7243(3) 0.0546(8) Uani 1 1 d . . .
H10 H 0.1766 0.3085 0.7220 0.066 Uiso 1 1 calc R . .
C13 C 0.2941(2) 0.25093(13) 0.72628(19) 0.0430(6) Uani 1 1 d . . .
C14 C 0.2316(2) 0.19828(13) 0.7229(2) 0.0441(6) Uani 1 1 d . . .
C15 C 0.2771(3) 0.14554(15) 0.7189(3) 0.0559(8) Uani 1 1 d . . .
H11 H 0.3488 0.1428 0.7143 0.067 Uiso 1 1 calc R . .
C16 C 0.1256(3) 0.19955(17) 0.7235(3) 0.0627(9) Uani 1 1 d . . .
H12 H 0.0908 0.2350 0.7223 0.075 Uiso 1 1 calc R . .
C17 C 0.2189(3) 0.09674(16) 0.7215(3) 0.0585(8) Uani 1 1 d . . .
H13 H 0.2510 0.0607 0.7194 0.070 Uiso 1 1 calc R . .
C18 C 0.0707(3) 0.15003(18) 0.7259(3) 0.0650(9) Uani 1 1 d . . .
H14 H -0.0017 0.1516 0.7267 0.078 Uiso 1 1 calc R . .
C19 C 0.0617(3) 0.04633(17) 0.7424(3) 0.0602(9) Uani 1 1 d . . .
H15 H 0.0775 0.0175 0.6947 0.072 Uiso 1 1 calc R . .
H16 H -0.0135 0.0533 0.7332 0.072 Uiso 1 1 calc R . .
C20 C 0.0936(2) 0.02465(15) 0.8429(2) 0.0509(7) Uani 1 1 d . . .
C21 C 0.1296(3) -0.03092(16) 0.8579(2) 0.0580(8) Uani 1 1 d . . .
H17 H 0.1361 -0.0550 0.8043 0.070 Uiso 1 1 calc R . .
C22 C 0.0877(3) 0.05980(16) 0.9220(3) 0.0548(8) Uani 1 1 d . . .
H18 H 0.0642 0.0978 0.9125 0.066 Uiso 1 1 calc R . .
C23 C 0.1559(3) -0.05101(17) 0.9520(3) 0.0586(8) Uani 1 1 d . . .
H19 H 0.1791 -0.0890 0.9623 0.070 Uiso 1 1 calc R . .
C24 C 0.1159(3) 0.03961(17) 1.0150(2) 0.0558(8) Uani 1 1 d . . .
H20 H 0.1130 0.0642 1.0686 0.067 Uiso 1 1 calc R . .
C25 C 0.1482(2) -0.01568(16) 1.0305(2) 0.0511(7) Uani 1 1 d . . .
C26 C 0.1748(3) -0.03747(19) 1.1328(3) 0.0604(9) Uani 1 1 d . . .
C27 C 0.4701(3) 0.33173(13) 0.0094(2) 0.0452(6) Uani 1 1 d . . .
C28 C 0.3739(3) 0.29653(13) -0.01008(19) 0.0456(7) Uani 1 1 d . . .
C29 C 0.3857(3) 0.23789(15) -0.0126(2) 0.0585(9) Uani 1 1 d . . .
H21 H 0.4527 0.2217 -0.0069 0.070 Uiso 1 1 calc R . .
C30 C 0.2988(4) 0.20261(17) -0.0237(3) 0.0741(13) Uani 1 1 d . . .
H22 H 0.3071 0.1626 -0.0248 0.089 Uiso 1 1 calc R . .
C31 C 0.2023(4) 0.22547(18) -0.0328(3) 0.0683(11) Uani 1 1 d . . .
H23 H 0.1437 0.2013 -0.0395 0.082 Uiso 1 1 calc R . .
C32 C 0.1894(3) 0.28339(17) -0.0325(3) 0.0631(9) Uani 1 1 d . . .
H24 H 0.1219 0.2989 -0.0396 0.076 Uiso 1 1 calc R . .
C33 C 0.2746(3) 0.31996(14) -0.0217(2) 0.0484(7) Uani 1 1 d . . .
C34 C 0.2579(3) 0.38304(15) -0.0288(2) 0.0550(8) Uani 1 1 d . . .
H1W H 0.438(4) 0.468(2) 0.1497(19) 0.097(17) Uiso 1 1 d D . .
H2W H 0.413(3) 0.4512(17) 0.056(3) 0.076(13) Uiso 1 1 d D . .
H3W H 0.670(3) 0.5225(14) 0.125(2) 0.059(11) Uiso 1 1 d D . .
H4W H 0.717(2) 0.492(2) 0.200(3) 0.100(18) Uiso 1 1 d D . .
H5W H 0.738(8) 0.401(3) 0.143(6) 0.20(4) Uiso 1 1 d D . .
H6W H 0.728(5) 0.389(3) 0.237(2) 0.13(2) Uiso 1 1 d D . .
H7W H 0.583(4) 0.4536(19) -0.030(4) 0.098(17) Uiso 1 1 d D . .
H8W H 0.606(5) 0.3944(13) -0.022(4) 0.12(2) Uiso 1 1 d 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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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'
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
O1 Ni1 O2W 90.34(10) . . ?
O1 Ni1 O3W 85.17(10) . . ?
O2W Ni1 O3W 91.50(10) . . ?
O1 Ni1 O5 89.74(9) . . ?
O2W Ni1 O5 172.22(9) . . ?
O3W Ni1 O5 96.27(10) . . ?
O1 Ni1 O4W 176.29(9) . . ?
O2W Ni1 O4W 89.53(10) . . ?
O3W Ni1 O4W 91.13(10) . . ?
O5 Ni1 O4W 90.88(9) . . ?
O1 Ni1 O1W 92.66(9) . . ?
O2W Ni1 O1W 86.17(9) . . ?
O3W Ni1 O1W 176.81(9) . . ?
O5 Ni1 O1W 86.05(9) . . ?
O4W Ni1 O1W 91.03(9) . . ?
C1 O1 Ni1 128.1(2) . . ?
C27 O5 Ni1 127.8(2) . . ?
C10 N1 C9 120.3(3) . . ?
C10 N1 C8 120.1(3) . . ?
C9 N1 C8 119.5(3) . . ?
C18 N2 C17 120.4(3) . . ?
C18 N2 C19 121.5(3) . . ?
C17 N2 C19 117.9(3) . . ?
O2 C1 O1 125.2(3) . . ?
O2 C1 C2 118.3(3) . . ?
O1 C1 C2 116.4(3) . . ?
C3 C2 C4 119.3(3) . . ?
C3 C2 C1 120.6(3) . . ?
C4 C2 C1 120.2(3) . . ?
C5 C3 C2 120.5(3) . . ?
C6 C4 C2 119.8(3) . . ?
C3 C5 C7 120.4(3) . . ?
C4 C6 C7 120.7(3) . . ?
C5 C7 C6 119.4(3) . . ?
C5 C7 C8 120.4(3) . . ?
C6 C7 C8 120.2(3) . . ?
N1 C8 C7 108.3(2) . . ?
N1 C9 C11 121.0(3) . . ?
N1 C10 C12 120.8(3) . . ?
C9 C11 C13 120.6(3) . . ?
C10 C12 C13 120.4(3) . . ?
C11 C13 C12 116.9(3) . . ?
C11 C13 C14 121.1(3) . . ?
C12 C13 C14 122.0(3) . . ?
C15 C14 C16 117.1(3) . . ?
C15 C14 C13 120.9(3) . . ?
C16 C14 C13 122.0(3) . . ?
C17 C15 C14 120.3(3) . . ?
C18 C16 C14 120.5(4) . . ?
N2 C17 C15 120.5(3) . . ?
N2 C18 C16 120.9(3) . . ?
N2 C19 C20 109.8(3) . . ?
C22 C20 C21 119.3(3) . . ?
C22 C20 C19 120.2(3) . . ?
C21 C20 C19 120.5(3) . . ?
C20 C21 C23 119.8(3) . . ?
C24 C22 C20 120.3(4) . . ?
C25 C23 C21 120.3(4) . . ?
C25 C24 C22 120.7(3) . . ?
C24 C25 C23 119.6(3) . . ?
C24 C25 C26 119.8(3) . . ?
C23 C25 C26 120.6(3) . . ?
O3 C26 O4 124.5(3) . . ?
O3 C26 C25 118.8(4) . . ?
O4 C26 C25 116.7(4) . . ?
O6 C27 O5 125.6(3) . . ?
O6 C27 C28 117.5(3) . . ?
O5 C27 C28 116.8(3) . . ?
C29 C28 C33 119.5(3) . . ?
C29 C28 C27 117.3(3) . . ?
C33 C28 C27 123.2(3) . . ?
C28 C29 C30 120.0(4) . . ?
C31 C30 C29 120.4(4) . . ?
C30 C31 C32 120.2(4) . . ?
C31 C32 C33 120.9(4) . . ?
C32 C33 C28 118.9(3) . . ?
C32 C33 C34 119.5(3) . . ?
C28 C33 C34 121.5(3) . . ?
O7 C34 O8 123.5(4) . . ?
O7 C34 C33 118.2(3) . . ?
O8 C34 C33 118.4(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 O1 2.042(2) . ?
Ni1 O2W 2.056(2) . ?
Ni1 O3W 2.066(2) . ?
Ni1 O5 2.079(2) . ?
Ni1 O4W 2.081(2) . ?
Ni1 O1W 2.101(2) . ?
O1 C1 1.255(4) . ?
O2 C1 1.242(4) . ?
O3 C26 1.241(5) . ?
O4 C26 1.254(5) . ?
O5 C27 1.263(4) . ?
O6 C27 1.255(4) . ?
O7 C34 1.252(4) . ?
O8 C34 1.255(5) . ?
N1 C10 1.342(4) . ?
N1 C9 1.348(4) . ?
N1 C8 1.501(4) . ?
N2 C18 1.329(5) . ?
N2 C17 1.342(5) . ?
N2 C19 1.486(4) . ?
C1 C2 1.508(4) . ?
C2 C3 1.389(4) . ?
C2 C4 1.403(4) . ?
C3 C5 1.385(4) . ?
C4 C6 1.384(4) . ?
C5 C7 1.387(4) . ?
C6 C7 1.390(4) . ?
C7 C8 1.518(4) . ?
C9 C11 1.357(5) . ?
C10 C12 1.367(5) . ?
C11 C13 1.398(4) . ?
C12 C13 1.399(5) . ?
C13 C14 1.484(4) . ?
C14 C15 1.382(5) . ?
C14 C16 1.388(5) . ?
C15 C17 1.382(5) . ?
C16 C18 1.373(5) . ?
C19 C20 1.502(4) . ?
C20 C22 1.390(5) . ?
C20 C21 1.398(5) . ?
C21 C23 1.399(5) . ?
C22 C24 1.389(5) . ?
C23 C25 1.389(5) . ?
C24 C25 1.378(5) . ?
C25 C26 1.517(4) . ?
C27 C28 1.504(5) . ?
C28 C29 1.391(5) . ?
C28 C33 1.403(5) . ?
C29 C30 1.403(6) . ?
C30 C31 1.365(7) . ?
C31 C32 1.374(6) . ?
C32 C33 1.403(5) . ?
C33 C34 1.503(5) . ?
