#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:29:33 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179633 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/97/4509799.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4509799
loop_
_publ_author_name
'Ji, Cong-Min'
'Yang, Hui-Juan'
'Zhao, Chong-Chao'
'Tangoulis, Vassilis'
'Cui, Ai-Li'
'Kou, Hui-Zhong'
_publ_section_title
;
 Self-Assembly of Multidecker NiIIClusters from Preformed Ni4Decks
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4607
_journal_paper_doi               10.1021/cg900975y
_journal_volume                  9
_journal_year                    2009
_chemical_formula_sum            'C36 H38 Cl2 N20 Ni4 O12'
_chemical_formula_weight         1248.60
_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                101.92(3)
_cell_angle_beta                 101.18(3)
_cell_angle_gamma                112.71(3)
_cell_formula_units_Z            1
_cell_length_a                   10.444(2)
_cell_length_b                   11.355(2)
_cell_length_c                   11.697(2)
_cell_measurement_reflns_used    4166
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.17
_cell_volume                     1193.1(6)
_computing_cell_refinement       'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_data_collection       'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_data_reduction        'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XP (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.77
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'ω 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  0.0868
_diffrn_reflns_av_sigmaI/netI    0.1204
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9114
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    1.748
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR; Higashi, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.904
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1723
_refine_ls_R_factor_gt           0.0950
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1282P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2215
_refine_ls_wR_factor_ref         0.2589
_reflns_number_gt                2008
_reflns_number_total             4166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg900975ysup1.cif
_cod_data_source_block           Ni4
_cod_original_cell_volume        1193.1(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4509799
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 0.92816(14) 0.37447(13) 0.09206(11) 0.0572(5) Uani 1 1 d .
Ni2 Ni 1.28556(14) 0.45186(13) 0.18057(11) 0.0597(5) Uani 1 1 d .
Cl1 Cl 1.2557(5) 0.0779(4) 0.6458(3) 0.1027(11) Uani 1 1 d .
N2 N 1.1318(9) 0.2151(8) 0.3792(7) 0.067(2) Uani 1 1 d .
H2B H 1.0392 0.1888 0.3597 0.080 Uiso 1 1 calc R
H2C H 1.1732 0.1902 0.4340 0.080 Uiso 1 1 calc R
N5 N 0.8154(9) 0.4416(8) -0.0176(7) 0.060(2) Uani 1 1 d .
O7 O 1.1387(7) 0.4709(7) 0.0873(6) 0.0626(18) Uani 1 1 d .
C11 C 0.6160(11) 0.2947(10) 0.0245(8) 0.057(2) Uani 1 1 d .
O6 O 1.0092(7) 0.2918(7) 0.2079(6) 0.0640(18) Uani 1 1 d .
N1 N 1.4226(9) 0.4222(9) 0.2843(6) 0.060(2) Uani 1 1 d .
C12 C 0.6774(12) 0.3944(10) -0.0393(8) 0.061(3) Uani 1 1 d .
N3 N 1.1532(9) 0.3361(7) 0.2394(7) 0.055(2) Uani 1 1 d .
N4 N 0.7157(9) 0.2693(8) 0.0935(7) 0.060(2) Uani 1 1 d .
N6 N 1.4008(9) 0.5677(9) 0.1145(7) 0.066(2) Uani 1 1 d .
H6A H 1.4932 0.5943 0.1299 0.080 Uiso 1 1 calc R
N10 N 0.9680(9) 0.5323(8) 0.2429(8) 0.068(2) Uani 1 1 d .
C4 C 1.4514(12) 0.3109(11) 0.4348(9) 0.069(3) Uani 1 1 d .
H4A H 1.4112 0.2569 0.4807 0.083 Uiso 1 1 calc R
C5 C 1.3664(11) 0.3427(10) 0.3529(8) 0.057(3) Uani 1 1 d .
N8 N 0.8928(10) 0.2174(10) -0.0561(9) 0.080(3) Uani 1 1 d .
C6 C 1.2118(11) 0.2950(10) 0.3242(8) 0.056(2) Uani 1 1 d .
C7 C 0.6724(12) 0.1836(11) 0.1554(9) 0.070(3) Uani 1 1 d .
H7A H 0.7415 0.1683 0.2051 0.085 Uiso 1 1 calc R
C8 C 0.5287(13) 0.1167(12) 0.1486(10) 0.079(3) Uani 1 1 d .
H8A H 0.5004 0.0545 0.1905 0.095 Uiso 1 1 calc R
C18 C 1.0438(12) 0.5581(12) 0.3628(10) 0.079(3) Uani 1 1 d .
H18A H 1.0811 0.5030 0.3899 0.094 Uiso 1 1 calc R
C3 C 1.5972(14) 0.3615(13) 0.4466(10) 0.082(4) Uani 1 1 d .
H3A H 1.6568 0.3406 0.5006 0.098 Uiso 1 1 calc R
C10 C 0.4691(13) 0.2325(12) 0.0171(9) 0.076(3) Uani 1 1 d .
H10A H 0.4013 0.2520 -0.0291 0.091 Uiso 1 1 calc R
N9 N 0.9866(11) 0.7177(9) 0.3606(10) 0.087(3) Uani 1 1 d .
H9B H 0.9772 0.7903 0.3824 0.105 Uiso 1 1 calc R
C2 C 1.6569(13) 0.4427(12) 0.3796(10) 0.078(3) Uani 1 1 d .
H2A H 1.7559 0.4769 0.3877 0.094 Uiso 1 1 calc R
C17 C 0.9339(13) 0.6317(12) 0.2472(11) 0.078(3) Uani 1 1 d .
H17A H 0.8797 0.6415 0.1799 0.093 Uiso 1 1 calc R
C16 C 1.0567(14) 0.6718(14) 0.4347(11) 0.090(4) Uani 1 1 d .
H16A H 1.1041 0.7111 0.5185 0.108 Uiso 1 1 calc R
C9 C 0.4279(13) 0.1431(12) 0.0791(11) 0.085(4) Uani 1 1 d .
H9A H 0.3303 0.0992 0.0744 0.102 Uiso 1 1 calc R
C1 C 1.5676(12) 0.4715(11) 0.3014(9) 0.068(3) Uani 1 1 d .
H1A H 1.6081 0.5279 0.2574 0.081 Uiso 1 1 calc R
C14 C 0.7954(14) 0.1706(13) -0.1683(11) 0.085(4) Uani 1 1 d .
H14A H 0.7274 0.2012 -0.1938 0.102 Uiso 1 1 calc R
C15 C 0.9666(17) 0.1411(14) -0.0654(13) 0.103(4) Uani 1 1 d .
H15A H 1.0408 0.1503 -0.0004 0.124 Uiso 1 1 calc R
C13 C 0.924(2) 0.0541(18) -0.1738(18) 0.135(7) Uani 1 1 d .
H13A H 0.9602 -0.0058 -0.2009 0.162 Uiso 1 1 calc R
O5 O 1.2054(15) -0.0247(13) 0.6871(13) 0.195(6) Uani 1 1 d .
N7 N 0.8147(19) 0.0719(16) -0.2363(13) 0.146(6) Uani 1 1 d .
H7B H 0.7632 0.0257 -0.3111 0.175 Uiso 1 1 calc R
O4 O 1.4087(16) 0.1089(17) 0.6794(18) 0.236(8) Uani 1 1 d .
O3 O 1.2612(16) 0.1979(12) 0.7000(16) 0.225(8) Uani 1 1 d .
O2 O 1.185(3) 0.0414(15) 0.5308(12) 0.326(16) 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'
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'
Cl Cl 0.1484 0.1585 '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
O6 Ni1 N5 170.4(3) . .
O6 Ni1 O7 85.7(3) . .
N5 Ni1 O7 103.8(3) . .
O6 Ni1 N8 89.9(3) . .
N5 Ni1 N8 91.2(4) . .
O7 Ni1 N8 88.5(3) . .
O6 Ni1 N4 93.1(3) . .
N5 Ni1 N4 77.4(3) . .
O7 Ni1 N4 177.5(3) . .
N8 Ni1 N4 89.3(3) . .
O6 Ni1 N10 89.1(3) . .
N5 Ni1 N10 89.9(3) . .
O7 Ni1 N10 90.6(3) . .
N8 Ni1 N10 178.7(4) . .
N4 Ni1 N10 91.6(3) . .
O7 Ni2 N6 84.5(3) . .
O7 Ni2 N3 89.9(3) . .
N6 Ni2 N3 174.4(3) . .
O7 Ni2 N1 173.9(3) . .
N6 Ni2 N1 101.5(4) . .
N3 Ni2 N1 84.1(4) . .
O2 Cl1 O5 108.7(10) . .
O2 Cl1 O3 107.3(10) . .
O5 Cl1 O3 121.6(12) . .
O2 Cl1 O4 118.7(14) . .
O5 Cl1 O4 99.7(10) . .
O3 Cl1 O4 101.3(9) . .
C6 N2 H2B 120.0 . .
C6 N2 H2C 120.0 . .
H2B N2 H2C 120.0 . .
C12 N5 O7 109.6(7) . 2_765
C12 N5 Ni1 119.5(7) . .
O7 N5 Ni1 130.7(6) 2_765 .
N5 O7 Ni2 113.8(5) 2_765 .
N5 O7 Ni1 125.4(5) 2_765 .
Ni2 O7 Ni1 120.7(3) . .
N4 C11 C10 121.4(9) . .
N4 C11 C12 114.2(9) . .
C10 C11 C12 124.3(9) . .
N3 O6 Ni1 115.3(5) . .
C1 N1 C5 117.2(8) . .
C1 N1 Ni2 128.4(7) . .
C5 N1 Ni2 114.3(7) . .
N5 C12 N6 121.1(9) . 2_765
N5 C12 C11 114.1(9) . .
N6 C12 C11 124.8(10) 2_765 .
C6 N3 O6 117.1(8) . .
C6 N3 Ni2 114.8(7) . .
O6 N3 Ni2 128.1(6) . .
C7 N4 C11 118.9(9) . .
C7 N4 Ni1 126.3(7) . .
C11 N4 Ni1 114.8(7) . .
C12 N6 Ni2 110.9(7) 2_765 .
C12 N6 H6A 124.5 2_765 .
Ni2 N6 H6A 124.5 . .
C17 N10 C18 103.7(9) . .
C17 N10 Ni1 129.3(8) . .
C18 N10 Ni1 126.9(7) . .
C3 C4 C5 117.8(11) . .
C3 C4 H4A 121.1 . .
C5 C4 H4A 121.1 . .
N1 C5 C4 122.4(10) . .
N1 C5 C6 111.6(8) . .
C4 C5 C6 126.0(10) . .
C14 N8 C15 103.7(11) . .
C14 N8 Ni1 127.8(9) . .
C15 N8 Ni1 128.4(9) . .
N3 C6 N2 122.2(9) . .
N3 C6 C5 115.1(9) . .
N2 C6 C5 122.7(8) . .
N4 C7 C8 122.1(10) . .
N4 C7 H7A 119.0 . .
C8 C7 H7A 119.0 . .
C7 C8 C9 118.9(11) . .
C7 C8 H8A 120.6 . .
C9 C8 H8A 120.6 . .
C16 C18 N10 111.2(11) . .
C16 C18 H18A 124.4 . .
N10 C18 H18A 124.4 . .
C4 C3 C2 121.0(11) . .
C4 C3 H3A 119.5 . .
C2 C3 H3A 119.5 . .
C9 C10 C11 118.2(11) . .
C9 C10 H10A 120.9 . .
C11 C10 H10A 120.9 . .
C17 N9 C16 108.5(9) . .
C17 N9 H9B 125.8 . .
C16 N9 H9B 125.8 . .
C1 C2 C3 118.3(12) . .
C1 C2 H2A 120.8 . .
C3 C2 H2A 120.8 . .
N10 C17 N9 111.4(11) . .
N10 C17 H17A 124.3 . .
N9 C17 H17A 124.3 . .
C18 C16 N9 105.2(10) . .
C18 C16 H16A 127.4 . .
N9 C16 H16A 127.4 . .
C10 C9 C8 120.5(11) . .
C10 C9 H9A 119.7 . .
C8 C9 H9A 119.7 . .
N1 C1 C2 123.2(11) . .
N1 C1 H1A 118.4 . .
C2 C1 H1A 118.4 . .
N7 C14 N8 107.3(13) . .
N7 C14 H14A 126.3 . .
N8 C14 H14A 126.3 . .
C13 C15 N8 114.0(16) . .
C13 C15 H15A 123.0 . .
N8 C15 H15A 123.0 . .
N7 C13 C15 103.2(15) . .
N7 C13 H13A 128.4 . .
C15 C13 H13A 128.4 . .
C14 N7 C13 111.8(14) . .
C14 N7 H7B 124.1 . .
C13 N7 H7B 124.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O6 2.032(6) .
Ni1 N5 2.031(7) .
Ni1 O7 2.062(7) .
Ni1 N8 2.071(10) .
Ni1 N4 2.080(8) .
Ni1 N10 2.082(8) .
Ni2 O7 1.815(6) .
Ni2 N6 1.826(8) .
Ni2 N3 1.859(8) .
Ni2 N1 1.871(7) .
Cl1 O2 1.295(11) .
Cl1 O5 1.314(11) .
Cl1 O3 1.353(12) .
Cl1 O4 1.448(15) .
N2 C6 1.342(12) .
N2 H2B 0.8600 .
N2 H2C 0.8600 .
N5 C12 1.278(12) .
N5 O7 1.414(10) 2_765
O7 N5 1.414(10) 2_765
C11 N4 1.350(11) .
C11 C10 1.395(14) .
C11 C12 1.492(13) .
O6 N3 1.332(9) .
N1 C1 1.352(13) .
N1 C5 1.370(12) .
C12 N6 1.332(11) 2_765
N3 C6 1.322(11) .
N4 C7 1.325(13) .
N6 C12 1.332(11) 2_765
N6 H6A 0.8600 .
N10 C17 1.302(12) .
N10 C18 1.379(12) .
C4 C3 1.371(15) .
C4 C5 1.378(13) .
C4 H4A 0.9300 .
C5 C6 1.433(13) .
N8 C14 1.348(14) .
N8 C15 1.366(16) .
C7 C8 1.372(15) .
C7 H7A 0.9300 .
C8 C9 1.368(15) .
C8 H8A 0.9300 .
C18 C16 1.329(15) .
C18 H18A 0.9300 .
C3 C2 1.377(16) .
C3 H3A 0.9300 .
C10 C9 1.352(15) .
C10 H10A 0.9300 .
N9 C17 1.335(13) .
N9 C16 1.339(14) .
N9 H9B 0.8600 .
C2 C1 1.357(13) .
C2 H2A 0.9300 .
C17 H17A 0.9300 .
C16 H16A 0.9300 .
C9 H9A 0.9300 .
C1 H1A 0.9300 .
C14 N7 1.341(17) .
C14 H14A 0.9300 .
C15 C13 1.305(18) .
C15 H15A 0.9300 .
C13 N7 1.34(2) .
C13 H13A 0.9300 .
N7 H7B 0.8600 .
