#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:21:16 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180389 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/58/7205817.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_7205817
loop_
_publ_author_name
'Zhang, Wen-Hua'
'Sulaiman, Norlela Binte'
'Tio, P. X. Shaun'
'Hor, T. S. Andy'
_publ_section_title
;
 Nuclearity growth towards Ni(ii) cubane in self-assembly with
 2-hydroxymethyl pyridine (hmpH) and 5-ethoxycarbonyl-2-hydroxymethyl
 pyridine (5-ehmpH)
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              2915
_journal_paper_doi               10.1039/c0ce00831a
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C36 H48 Br4 N4 Ni4 O16'
_chemical_formula_weight         1347.26
_chemical_name_systematic
;
?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1496(4)
_cell_length_b                   17.1496(4)
_cell_length_c                   16.3976(8)
_cell_measurement_reflns_used    7735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.38
_cell_volume                     4822.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16743
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    4.920
_exptl_absorpt_correction_T_max  0.5065
_exptl_absorpt_correction_T_min  0.3020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0429P)²+4.4986P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                2485
_reflns_number_total             2765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00831a.txt
_cod_data_source_block           Ni4(ehmp)4Br4(H2O)4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not Measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               7205817
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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 0.508969(15) 0.657389(15) 0.560398(15) 0.01528(9) Uani 1 1 d . . .
Br1 Br 0.622315(13) 0.564329(13) 0.547394(14) 0.02445(9) Uani 1 1 d . . .
O1 O 0.42336(8) 0.74018(8) 0.56567(8) 0.0160(3) Uani 1 1 d . . .
O2 O 0.60081(9) 0.59144(10) 0.24459(9) 0.0250(3) Uani 1 1 d . . .
O3 O 0.49897(10) 0.59432(12) 0.15823(10) 0.0358(4) Uani 1 1 d . . .
O4 O 0.43866(10) 0.56191(10) 0.58036(11) 0.0235(3) Uani 1 1 d . . .
H41 H 0.4238(17) 0.5339(17) 0.5478(18) 0.022(7) Uiso 1 1 d . . .
H42 H 0.396(2) 0.5702(17) 0.6079(19) 0.036(8) Uiso 1 1 d . . .
N1 N 0.47477(10) 0.65984(10) 0.43972(10) 0.0174(3) Uani 1 1 d . . .
C1 C 0.51245(12) 0.63117(12) 0.37452(13) 0.0186(4) Uani 1 1 d . . .
H1 H 0.5613 0.6061 0.3823 0.022 Uiso 1 1 calc R . .
C2 C 0.48249(13) 0.63692(13) 0.29600(13) 0.0205(4) Uani 1 1 d . . .
C3 C 0.41146(13) 0.67368(14) 0.28446(13) 0.0233(5) Uani 1 1 d . . .
H3 H 0.3900 0.6789 0.2313 0.028 Uiso 1 1 calc R . .
C4 C 0.37215(13) 0.70280(13) 0.35198(13) 0.0218(4) Uani 1 1 d . . .
H4A H 0.3230 0.7277 0.3457 0.026 Uiso 1 1 calc R . .
C5 C 0.40544(12) 0.69503(12) 0.42879(12) 0.0176(4) Uani 1 1 d . . .
C6 C 0.36628(12) 0.72575(13) 0.50524(12) 0.0189(4) Uani 1 1 d . . .
H6A H 0.3379 0.7746 0.4926 0.023 Uiso 1 1 calc R . .
H6B H 0.3281 0.6870 0.5256 0.023 Uiso 1 1 calc R . .
C7 C 0.52713(13) 0.60562(14) 0.22477(13) 0.0233(4) Uani 1 1 d . . .
C8 C 0.65170(14) 0.56220(15) 0.17997(14) 0.0276(5) Uani 1 1 d . . .
H8A H 0.6471 0.5952 0.1307 0.033 Uiso 1 1 calc R . .
H8B H 0.6373 0.5081 0.1654 0.033 Uiso 1 1 calc R . .
C9 C 0.73288(15) 0.56496(16) 0.21261(16) 0.0319(5) Uani 1 1 d . . .
H9A H 0.7456 0.6185 0.2285 0.048 Uiso 1 1 calc R . .
H9B H 0.7694 0.5474 0.1704 0.048 Uiso 1 1 calc R . .
H9C H 0.7369 0.5307 0.2603 0.048 Uiso 1 1 calc R . .
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'
Br Br -0.2901 2.4595 '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 O1 82.56(6) . 12_767 ?
O1 Ni1 O4 97.18(6) . . ?
O1 Ni1 O4 87.30(6) 12_767 . ?
O1 Ni1 N1 79.76(6) . . ?
O1 Ni1 N1 161.67(7) 12_767 . ?
O4 Ni1 N1 90.13(7) . . ?
O1 Ni1 O1 79.33(6) . 6_564 ?
O1 Ni1 O1 81.03(6) 12_767 6_564 ?
O4 Ni1 O1 168.14(6) . 6_564 ?
N1 Ni1 O1 100.30(6) . 6_564 ?
O1 Ni1 Br1 174.76(4) . . ?
O1 Ni1 Br1 99.36(4) 12_767 . ?
O4 Ni1 Br1 87.80(5) . . ?
N1 Ni1 Br1 98.67(5) . . ?
O1 Ni1 Br1 96.11(4) 6_564 . ?
C6 O1 Ni1 110.24(11) . . ?
C6 O1 Ni1 127.08(12) . 15_566 ?
Ni1 O1 Ni1 98.21(6) . 15_566 ?
C6 O1 Ni1 119.88(12) . 6_564 ?
Ni1 O1 Ni1 100.47(6) . 6_564 ?
Ni1 O1 Ni1 96.21(6) 15_566 6_564 ?
C7 O2 C8 116.99(18) . . ?
Ni1 O4 H41 126(2) . . ?
Ni1 O4 H42 116(2) . . ?
H41 O4 H42 101(3) . . ?
C1 N1 C5 118.93(18) . . ?
C1 N1 Ni1 128.25(15) . . ?
C5 N1 Ni1 112.82(13) . . ?
N1 C1 C2 122.3(2) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C3 C2 C1 119.0(2) . . ?
C3 C2 C7 120.45(19) . . ?
C1 C2 C7 120.6(2) . . ?
C2 C3 C4 118.8(2) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C3 C4 C5 119.3(2) . . ?
C3 C4 H4A 120.4 . . ?
C5 C4 H4A 120.4 . . ?
N1 C5 C4 121.80(19) . . ?
N1 C5 C6 115.92(17) . . ?
C4 C5 C6 122.28(19) . . ?
O1 C6 C5 109.47(16) . . ?
O1 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
O1 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?
O3 C7 O2 124.9(2) . . ?
O3 C7 C2 123.9(2) . . ?
O2 C7 C2 111.21(18) . . ?
O2 C8 C9 106.63(19) . . ?
O2 C8 H8A 110.4 . . ?
C9 C8 H8A 110.4 . . ?
O2 C8 H8B 110.4 . . ?
C9 C8 H8B 110.4 . . ?
H8A C8 H8B 108.6 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
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 2.0442(15) . ?
Ni1 O1 2.0507(14) 12_767 ?
Ni1 O4 2.0596(17) . ?
Ni1 N1 2.0644(17) . ?
Ni1 O1 2.1072(15) 6_564 ?
Ni1 Br1 2.5241(3) . ?
O1 C6 1.415(2) . ?
O1 Ni1 2.0507(14) 15_566 ?
O1 Ni1 2.1072(15) 6_564 ?
O2 C7 1.327(3) . ?
O2 C8 1.461(3) . ?
O3 C7 1.209(3) . ?
O4 H41 0.76(3) . ?
O4 H42 0.87(3) . ?
N1 C1 1.342(3) . ?
N1 C5 1.345(3) . ?
C1 C2 1.390(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.385(3) . ?
C2 C7 1.496(3) . ?
C3 C4 1.389(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(3) . ?
C4 H4A 0.9500 . ?
C5 C6 1.517(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C8 C9 1.492(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
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
O4 H42 Br1 0.87(3) 2.31(3) 3.1363(18) 158(3) 15_566
O4 H41 Br1 0.76(3) 2.43(3) 3.1889(17) 175(3) 9_666
