#------------------------------------------------------------------------------
#$Date: 2017-07-11 15:10:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/12/7201242.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_7201242
loop_
_publ_author_name
'Colacio, Enrique'
'Aouryaghal, Hakima'
'Mota, Antonio J.'
'Cano, Joan'
'Sillanpää, Reijo'
'Rodríguez-Diéguez, A.'
_publ_section_title
;
 Anion encapsulation promoted by anion⋯π interactions in
 rationally designed hexanuclear antiferromagnetic wheels: synthesis,
 structure and magnetic properties
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2054
_journal_paper_doi               10.1039/b906382j
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C66 H114 B F6 N24 Ni6 O12'
_chemical_formula_weight         1912.88
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 130.773(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   23.206(5)
_cell_length_b                   20.746(5)
_cell_length_c                   16.193(5)
_cell_measurement_reflns_used    6028
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.61
_cell_measurement_theta_min      2.52
_cell_volume                     5904(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'Bruker SHELXTL)'
_computing_publication_material  'publCIF (Westrip, 2007)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.1160
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34133
_diffrn_reflns_theta_full        28.18
_diffrn_reflns_theta_max         28.18
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2002
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         7074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0480P)²+2.3724P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.1810
_reflns_number_gt                4736
_reflns_number_total             7074
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b906382j.txt
_cod_data_source_block           ar190
_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 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'contr' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7201242
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.0000 0.23396(3) 0.0000 0.05398(19) Uani 1 2 d S . .
Ni2 Ni 0.26223(2) 0.366935(18) 0.32525(4) 0.05773(17) Uani 1 1 d . . .
N1A N 0.07054(15) 0.30722(12) 0.0136(2) 0.0541(6) Uani 1 1 d . . .
C2A C 0.0653(2) 0.33972(18) -0.0616(3) 0.0692(9) Uani 1 1 d . . .
H2A H 0.0250 0.3316 -0.1351 0.083 Uiso 1 1 calc R . .
C3A C 0.1200(2) 0.3862(2) -0.0314(3) 0.0769(10) Uani 1 1 d . . .
H3A H 0.1168 0.4091 -0.0836 0.092 Uiso 1 1 calc R . .
C4A C 0.1782(2) 0.39662(18) 0.0777(3) 0.0688(9) Uani 1 1 d . . .
H4A H 0.2156 0.4268 0.0999 0.083 Uiso 1 1 calc R . .
N5A N 0.18244(15) 0.36413(12) 0.1531(2) 0.0558(7) Uani 1 1 d . . .
C6A C 0.12710(17) 0.32114(14) 0.1161(3) 0.0518(7) Uani 1 1 d . . .
C7A C 0.13321(17) 0.28345(14) 0.2016(3) 0.0530(7) Uani 1 1 d . . .
O8A O 0.08252(12) 0.24362(10) 0.16673(18) 0.0584(6) Uani 1 1 d . . .
O9A O 0.18830(13) 0.29665(10) 0.29800(18) 0.0619(6) Uani 1 1 d . . .
N1B N 0.19942(15) 0.44243(12) 0.3211(2) 0.0554(6) Uani 1 1 d . . .
C2B C 0.1396(2) 0.44332(18) 0.3178(3) 0.0665(9) Uani 1 1 d . . .
H2B H 0.1195 0.4047 0.3181 0.080 Uiso 1 1 calc R . .
C3B C 0.1087(3) 0.5000 0.3139(5) 0.0731(14) Uani 1 2 d S . .
H3B H 0.0663 0.5000 0.3086 0.088 Uiso 1 2 calc SR . .
C4B C 0.2252(2) 0.5000 0.3221(4) 0.0527(10) Uani 1 2 d S . .
C5B C 0.2936(2) 0.5000 0.3281(4) 0.0537(11) Uani 1 2 d S . .
O6B O 0.31739(12) 0.44652(10) 0.3288(2) 0.0625(6) Uani 1 1 d . . .
C1C C 0.3069(3) 0.2390(2) 0.2923(6) 0.148(3) Uani 1 1 d . . .
H1C1 H 0.2709 0.2415 0.2142 0.222 Uiso 1 1 calc R . .
H1C2 H 0.2818 0.2239 0.3178 0.222 Uiso 1 1 calc R . .
H1C3 H 0.3470 0.2097 0.3153 0.222 Uiso 1 1 calc R . .
C2C C 0.3693(3) 0.3276(3) 0.2836(6) 0.1197(19) Uani 1 1 d . . .
H2C1 H 0.4144 0.3041 0.3111 0.179 Uiso 1 1 calc R . .
H2C2 H 0.3812 0.3726 0.2994 0.179 Uiso 1 1 calc R . .
H2C3 H 0.3313 0.3216 0.2061 0.179 Uiso 1 1 calc R . .
N3C N 0.33900(18) 0.30284(16) 0.3377(4) 0.0914(12) Uani 1 1 d . . .
C4C C 0.4043(3) 0.2988(4) 0.4599(6) 0.144(3) Uani 1 1 d . . .
H4C1 H 0.4346 0.2609 0.4763 0.173 Uiso 1 1 calc R . .
H4C2 H 0.4366 0.3364 0.4838 0.173 Uiso 1 1 calc R . .
C5C C 0.3784(4) 0.2956(3) 0.5182(5) 0.137(2) Uani 1 1 d . . .
H5C1 H 0.4216 0.2922 0.5956 0.165 Uiso 1 1 calc R . .
H5C2 H 0.3471 0.2574 0.4961 0.165 Uiso 1 1 calc R . .
N6C N 0.3331(2) 0.35410(15) 0.4969(3) 0.0816(10) Uani 1 1 d . . .
C7C C 0.2913(3) 0.3420(3) 0.5349(4) 0.116(2) Uani 1 1 d . . .
H7C1 H 0.2441 0.3209 0.4783 0.175 Uiso 1 1 calc R . .
H7C2 H 0.2813 0.3822 0.5527 0.175 Uiso 1 1 calc R . .
H7C3 H 0.3213 0.3150 0.5984 0.175 Uiso 1 1 calc R . .
C8C C 0.3820(3) 0.4104(2) 0.5615(4) 0.125(2) Uani 1 1 d . . .
H8C1 H 0.4168 0.3995 0.6375 0.188 Uiso 1 1 calc R . .
H8C2 H 0.3508 0.4460 0.5494 0.188 Uiso 1 1 calc R . .
H8C3 H 0.4101 0.4223 0.5393 0.188 Uiso 1 1 calc R . .
C1D C -0.0458(4) 0.1655(3) 0.1150(5) 0.122(2) Uani 1 1 d . . .
H1D1 H -0.0812 0.1975 0.1007 0.183 Uiso 1 1 calc R . .
H1D2 H 0.0050 0.1786 0.1762 0.183 Uiso 1 1 calc R . .
H1D3 H -0.0568 0.1251 0.1311 0.183 Uiso 1 1 calc R . .
C2D C -0.1349(3) 0.1489(2) -0.0798(4) 0.1101(18) Uani 1 1 d . . .
H2D1 H -0.1511 0.1068 -0.0778 0.165 Uiso 1 1 calc R . .
H2D2 H -0.1413 0.1531 -0.1444 0.165 Uiso 1 1 calc R . .
H2D3 H -0.1650 0.1810 -0.0803 0.165 Uiso 1 1 calc R . .
N3D N -0.05272(18) 0.15809(15) 0.0189(3) 0.0769(9) Uani 1 1 d . . .
C4D C -0.0071(4) 0.1009(2) 0.0359(7) 0.142(3) Uani 1 1 d . . .
H4D1 H 0.0410 0.1009 0.1103 0.170 Uiso 1 1 calc R . .
H4D2 H -0.0343 0.0619 0.0252 0.170 Uiso 1 1 calc R . .
B1E B 0.0000 0.5000 0.0000 0.092(3) Uani 1 4 d S . .
F2E F 0.0286(8) 0.5000 -0.0593(11) 0.280(5) Uani 1 2 d S . .
F3E F 0.0440(6) 0.4588(5) 0.0654(6) 0.447(9) 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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
_geom_angle_publ_flag
O8A Ni1 O8A 168.83(12) . 2 ?
O8A Ni1 N3D 90.77(11) . . ?
O8A Ni1 N3D 97.48(11) 2 . ?
O8A Ni1 N3D 97.48(11) . 2 ?
O8A Ni1 N3D 90.77(11) 2 2 ?
N3D Ni1 N3D 85.0(2) . 2 ?
O8A Ni1 N1A 78.57(9) . . ?
O8A Ni1 N1A 93.43(10) 2 . ?
N3D Ni1 N1A 169.04(11) . . ?
N3D Ni1 N1A 93.86(12) 2 . ?
O8A Ni1 N1A 93.43(10) . 2 ?
O8A Ni1 N1A 78.57(9) 2 2 ?
N3D Ni1 N1A 93.86(12) . 2 ?
N3D Ni1 N1A 169.04(11) 2 2 ?
N1A Ni1 N1A 89.33(14) . 2 ?
O6B Ni2 O9A 169.04(9) . . ?
O6B Ni2 N1B 79.07(10) . . ?
O9A Ni2 N1B 93.27(10) . . ?
O6B Ni2 N5A 92.97(10) . . ?
O9A Ni2 N5A 78.98(10) . . ?
N1B Ni2 N5A 89.24(11) . . ?
O6B Ni2 N3C 91.81(11) . . ?
O9A Ni2 N3C 96.11(12) . . ?
N1B Ni2 N3C 170.54(12) . . ?
N5A Ni2 N3C 93.78(14) . . ?
O6B Ni2 N6C 97.32(12) . . ?
O9A Ni2 N6C 90.93(12) . . ?
N1B Ni2 N6C 93.59(13) . . ?
N5A Ni2 N6C 169.67(12) . . ?
N3C Ni2 N6C 85.02(16) . . ?
C6A N1A C2A 117.8(3) . . ?
C6A N1A Ni1 110.7(2) . . ?
C2A N1A Ni1 131.5(2) . . ?
N1A C2A C3A 120.7(4) . . ?
C4A C3A C2A 117.6(4) . . ?
N5A C4A C3A 121.3(3) . . ?
C6A N5A C4A 116.7(3) . . ?
C6A N5A Ni2 111.5(2) . . ?
C4A N5A Ni2 131.9(2) . . ?
N1A C6A N5A 126.0(3) . . ?
N1A C6A C7A 117.6(3) . . ?
N5A C6A C7A 116.4(3) . . ?
O8A C7A O9A 128.0(3) . . ?
O8A C7A C6A 115.8(3) . . ?
O9A C7A C6A 116.1(3) . . ?
C7A O8A Ni1 117.3(2) . . ?
C7A O9A Ni2 117.0(2) . . ?
C4B N1B C2B 115.5(3) . . ?
C4B N1B Ni2 111.7(2) . . ?
C2B N1B Ni2 132.9(2) . . ?
N1B C2B C3B 120.7(3) . . ?
C2B C3B C2B 120.1(5) 6_565 . ?
N1B C4B N1B 127.5(4) 6_565 . ?
N1B C4B C5B 116.2(2) 6_565 . ?
N1B C4B C5B 116.2(2) . . ?
O6B C5B O6B 127.7(4) . 6_565 ?
O6B C5B C4B 116.1(2) . . ?
O6B C5B C4B 116.1(2) 6_565 . ?
C5B O6B Ni2 116.9(2) . . ?
C1C N3C C4C 110.7(5) . . ?
C1C N3C C2C 106.9(5) . . ?
C4C N3C C2C 109.0(4) . . ?
C1C N3C Ni2 113.5(3) . . ?
C4C N3C Ni2 102.7(4) . . ?
C2C N3C Ni2 114.0(3) . . ?
C5C C4C N3C 112.1(4) . . ?
C4C C5C N6C 110.5(5) . . ?
C7C N6C C8C 104.5(4) . . ?
C7C N6C C5C 108.8(4) . . ?
C8C N6C C5C 112.3(4) . . ?
C7C N6C Ni2 114.2(3) . . ?
C8C N6C Ni2 113.9(3) . . ?
C5C N6C Ni2 103.3(3) . . ?
C1D N3D C4D 108.4(4) . . ?
C1D N3D C2D 109.0(4) . . ?
C4D N3D C2D 110.6(4) . . ?
C1D N3D Ni1 113.6(3) . . ?
C4D N3D Ni1 102.1(3) . . ?
C2D N3D Ni1 113.0(3) . . ?
C4D C4D N3D 111.7(5) 2 . ?
F3E B1E F3E 180.0(7) 6_565 2 ?
F3E B1E F3E 90.9(11) 6_565 5_565 ?
F3E B1E F3E 89.1(11) 2 5_565 ?
F3E B1E F3E 89.1(11) 6_565 . ?
F3E B1E F3E 90.9(11) 2 . ?
F3E B1E F3E 180.0(7) 5_565 . ?
F3E B1E F2E 84.9(5) 6_565 5_565 ?
F3E B1E F2E 95.1(5) 2 5_565 ?
F3E B1E F2E 95.1(5) 5_565 5_565 ?
F3E B1E F2E 84.9(5) . 5_565 ?
F3E B1E F2E 95.1(5) 6_565 . ?
F3E B1E F2E 84.9(5) 2 . ?
F3E B1E F2E 84.9(5) 5_565 . ?
F3E B1E F2E 95.1(5) . . ?
F2E B1E F2E 180.0(7) 5_565 . ?
B1E F3E F3E 45.4(5) . 6_565 ?
B1E F3E F3E 44.6(5) . 2 ?
F3E F3E F3E 90.000(9) 6_565 2 ?
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 O8A 2.060(2) . ?
Ni1 O8A 2.060(2) 2 ?
Ni1 N3D 2.134(3) . ?
Ni1 N3D 2.134(3) 2 ?
Ni1 N1A 2.137(3) . ?
Ni1 N1A 2.137(3) 2 ?
Ni2 O6B 2.067(2) . ?
Ni2 O9A 2.068(2) . ?
Ni2 N1B 2.111(3) . ?
Ni2 N5A 2.112(3) . ?
Ni2 N3C 2.125(3) . ?
Ni2 N6C 2.129(4) . ?
N1A C6A 1.310(4) . ?
N1A C2A 1.327(5) . ?
C2A C3A 1.403(6) . ?
C3A C4A 1.369(6) . ?
C4A N5A 1.341(5) . ?
N5A C6A 1.341(4) . ?
C6A C7A 1.514(5) . ?
C7A O8A 1.232(4) . ?
C7A O9A 1.240(4) . ?
N1B C4B 1.332(3) . ?
N1B C2B 1.353(4) . ?
C2B C3B 1.357(5) . ?
C3B C2B 1.357(5) 6_565 ?
C4B N1B 1.332(3) 6_565 ?
C4B C5B 1.525(6) . ?
C5B O6B 1.236(3) . ?
C5B O6B 1.236(3) 6_565 ?
C1C N3C 1.460(6) . ?
C2C N3C 1.526(7) . ?
N3C C4C 1.518(8) . ?
C4C C5C 1.413(8) . ?
C5C N6C 1.492(7) . ?
N6C C7C 1.469(7) . ?
N6C C8C 1.482(5) . ?
C1D N3D 1.466(6) . ?
C2D N3D 1.499(5) . ?
N3D C4D 1.492(6) . ?
C4D C4D 1.398(12) 2 ?
B1E F3E 1.217(7) 6_565 ?
B1E F3E 1.217(7) 2 ?
B1E F3E 1.217(7) 5_565 ?
B1E F3E 1.217(7) . ?
B1E F2E 1.481(11) 5_565 ?
B1E F2E 1.481(11) . ?
F3E F3E 1.71(2) 6_565 ?
F3E F3E 1.734(17) 2 ?
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 0.159 -0.032 -0.045 2214 745 ' '
