#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:39:11 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178909 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/38/4113897.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_4113897
loop_
_publ_author_name
'Cheng-Yong Su'
'Yue-Peng Cai'
'Chun-Long Chen'
'Mark D. Smith'
'Wolfgang Kaim'
'Hans-Conrad zur Loye'
_publ_section_title
;
 Ligand-Directed Molecular Architectures: Self-Assembly of Two-Dimensional
 Rectangular Metallacycles and Three-Dimensional Trigonal or Tetragonal
 Prisms
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8595
_journal_page_last               8613
_journal_paper_doi               10.1021/ja034267k
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C100 H116 Cl4 N16 Ni2 O10'
_chemical_formula_weight         1961.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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            2
_cell_length_a                   15.301(2)
_cell_length_b                   15.301(2)
_cell_length_c                   23.303(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5455.7(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  CCD
_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  0.0954
_diffrn_reflns_av_sigmaI/netI    0.1779
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            10422
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         5.48
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       Block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.2125
_refine_ls_R_factor_gt           0.0798
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2398
_reflns_number_gt                1036
_reflns_number_total             3036
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034267ksi20030121_054932_06.cif
_cod_data_source_block           6
_cod_database_code               4113897
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
Ni1 Ni 0.0000 0.0000 0.16512(5) 0.0516(5) Uani 1 4 d S
N1 N 0.0890(3) 0.1024(3) 0.16258(17) 0.0540(12) Uani 1 1 d .
N2 N 0.2074(3) 0.1766(3) 0.13430(18) 0.0620(13) Uani 1 1 d .
C1 C 0.0947(4) 0.1805(3) 0.1945(2) 0.0555(14) Uani 1 1 d .
C2 C 0.0429(4) 0.2134(4) 0.2377(2) 0.0657(16) Uani 1 1 d .
H2A H -0.0059 0.1827 0.2503 0.079 Uiso 1 1 calc R
C3 C 0.0639(4) 0.2908(4) 0.2613(3) 0.0743(18) Uani 1 1 d .
H3A H 0.0295 0.3134 0.2907 0.089 Uiso 1 1 calc R
C4 C 0.1355(5) 0.3369(4) 0.2426(3) 0.085(2) Uani 1 1 d .
H4A H 0.1470 0.3909 0.2594 0.102 Uiso 1 1 calc R
C5 C 0.1917(4) 0.3071(4) 0.2000(3) 0.0795(19) Uani 1 1 d .
H5A H 0.2406 0.3384 0.1881 0.095 Uiso 1 1 calc R
C6 C 0.1691(4) 0.2276(4) 0.1769(2) 0.0628(16) Uani 1 1 d .
C7 C 0.1565(4) 0.1049(4) 0.1275(2) 0.0560(14) Uani 1 1 d .
H7A H 0.1682 0.0615 0.1006 0.067 Uiso 1 1 calc R
C8 C 0.2907(4) 0.1971(4) 0.1075(2) 0.0807(19) Uani 1 1 d .
H8A H 0.3373 0.1823 0.1341 0.097 Uiso 1 1 calc R
H8B H 0.2935 0.2596 0.1007 0.097 Uiso 1 1 calc R
C9 C 0.3066(4) 0.1502(5) 0.0516(2) 0.0674(17) Uani 1 1 d .
C10 C 0.3491(4) 0.0700(5) 0.0523(2) 0.079(2) Uani 1 1 d .
C11 C 0.3702(6) 0.0294(7) 0.0000 0.087(3) Uani 1 2 d S
H11A H 0.3982 -0.0246 0.0000 0.105 Uiso 1 2 calc SR
C12 C 0.2828(5) 0.1889(6) 0.0000 0.067(2) Uani 1 2 d S
C13 C 0.2313(7) 0.2744(6) 0.0000 0.095(3) Uani 1 2 d S
H13A H 0.2201 0.2920 -0.0388 0.143 Uiso 0.50 1 calc PR
H13B H 0.2645 0.3188 0.0192 0.143 Uiso 0.50 1 calc PR
H13C H 0.1768 0.2659 0.0197 0.143 Uiso 0.50 1 calc PR
C14 C 0.3741(5) 0.0218(5) 0.1070(3) 0.110(2) Uani 1 1 d .
H14A H 0.3565 0.0556 0.1397 0.166 Uiso 1 1 calc R
H14B H 0.4363 0.0133 0.1079 0.166 Uiso 1 1 calc R
H14C H 0.3453 -0.0340 0.1078 0.166 Uiso 1 1 calc R
Cl1 Cl 0.0000 0.0000 0.0756(3) 0.200(3) Uani 1 4 d S
Cl2 Cl 0.0000 0.0000 0.2633(3) 0.181(2) Uani 1 4 d S
O1W O 0.0390(3) 0.1544(3) 0.0000 0.0443(12) Uani 1 2 d S
O2W O 0.3858(8) 0.4236(8) 0.1435(7) 0.180(6) Uani 0.50 1 d P
O3W O 0.298(2) 0.483(2) 0.0958(14) 0.202(12) Uiso 0.25 1 d P
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'
Cl Cl 0.1484 0.1585 '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'
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
N1 Ni1 N1 89.954(7) 2 3
N1 Ni1 N1 176.7(2) 2 .
N1 Ni1 N1 89.954(7) 3 .
N1 Ni1 N1 89.954(7) 2 4
N1 Ni1 N1 176.7(2) 3 4
N1 Ni1 N1 89.954(7) . 4
N1 Ni1 Cl1 88.37(11) 2 .
N1 Ni1 Cl1 88.37(11) 3 .
N1 Ni1 Cl1 88.37(11) . .
N1 Ni1 Cl1 88.37(11) 4 .
N1 Ni1 Cl2 91.63(11) 2 .
N1 Ni1 Cl2 91.63(11) 3 .
N1 Ni1 Cl2 91.63(11) . .
N1 Ni1 Cl2 91.63(11) 4 .
Cl1 Ni1 Cl2 180.0 . .
C7 N1 C1 104.7(4) . .
C7 N1 Ni1 123.7(4) . .
C1 N1 Ni1 131.6(4) . .
C7 N2 C6 107.2(4) . .
C7 N2 C8 129.0(5) . .
C6 N2 C8 123.7(5) . .
C2 C1 C6 119.5(5) . .
C2 C1 N1 131.3(5) . .
C6 C1 N1 109.2(5) . .
C3 C2 C1 118.9(5) . .
C2 C3 C4 120.9(6) . .
C3 C4 C5 123.4(6) . .
C6 C5 C4 114.5(6) . .
C5 C6 N2 132.0(6) . .
C5 C6 C1 122.8(6) . .
N2 C6 C1 105.2(5) . .
N1 C7 N2 113.7(5) . .
N2 C8 C9 114.2(5) . .
C10 C9 C12 120.6(6) . .
C10 C9 C8 119.1(6) . .
C12 C9 C8 120.3(6) . .
C9 C10 C11 119.2(6) . .
C9 C10 C14 123.8(6) . .
C11 C10 C14 117.0(7) . .
C10 C11 C10 120.2(9) . 10
C9 C12 C9 120.0(9) . 10
C9 C12 C13 120.0(4) . .
C9 C12 C13 120.0(4) 10 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.076(4) 2
Ni1 N1 2.076(4) 3
Ni1 N1 2.076(4) .
Ni1 N1 2.076(4) 4
Ni1 Cl1 2.086(7) .
Ni1 Cl2 2.287(6) .
N1 C7 1.318(6) .
N1 C1 1.411(6) .
N2 C7 1.354(6) .
N2 C6 1.391(7) .
N2 C8 1.454(7) .
C1 C2 1.376(7) .
C1 C6 1.409(7) .
C2 C3 1.344(7) .
C3 C4 1.375(8) .
C4 C5 1.390(8) .
C5 C6 1.376(7) .
C8 C9 1.507(7) .
C9 C10 1.389(8) .
C9 C12 1.389(7) .
C10 C11 1.406(8) .
C10 C14 1.521(8) .
C11 C10 1.406(8) 10
C12 C9 1.389(7) 10
C12 C13 1.528(11) .
