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#$Date: 2016-03-22 11:13:47 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178890 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/19/4111916.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_4111916
loop_
_publ_author_name
'Cristian Saul Campos-Fernández'
'Brandi L. Schottel'
'Helen T. Chifotides'
'Jitendra K. Bera'
'John Bacsa'
'John M. Koomen'
'David H. Russell'
'Kim R. Dunbar'
_publ_contact_author_address
; 
Department of Chemistry
Texas A&M University
PO Box 30012 
College Station 
Texas 77842-3012 
USA
;
_publ_contact_author_email       dunbar@mail.chem.tamu.edu
_publ_contact_author_fax         (979)8457177
_publ_contact_author_name        'Kim Dunbar'
_publ_contact_author_phone       (979)8621485
_publ_section_title
;
 Anion Template Effect on the Self-Assembly and Interconversion of
 Metallacyclophanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12909
_journal_page_last               12923
_journal_paper_doi               10.1021/ja052108q
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C28 H32 N14 Ni2, 4(Cl O4)'
_chemical_formula_sum            'C28 H32 Cl4 N14 Ni2 O16'
_chemical_formula_weight         1079.90
_chemical_name_common            '[Ni2(bptz)(CH3CN)8][ClO4]4'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             'October 24 2004'
_audit_creation_method
;
SHELXL-97, PLATON, and text editor.
;
_cell_angle_alpha                98.355(5)
_cell_angle_beta                 104.675(5)
_cell_angle_gamma                97.317(5)
_cell_formula_units_Z            1
_cell_length_a                   8.639(5)
_cell_length_b                   10.856(5)
_cell_length_c                   12.362(5)
_cell_measurement_temperature    110(2)
_cell_volume                     1093.2(9)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.826
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_device_type  'SMART 1K CCD'
_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  0.0349
_diffrn_reflns_av_sigmaI/netI    0.1151
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4421
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         4.21
_exptl_absorpt_coefficient_mu    1.188
_exptl_absorpt_correction_T_max  0.8904
_exptl_absorpt_correction_T_min  0.6415
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       needle
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         3362
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1285
_refine_ls_R_factor_gt           0.0612
_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)+(0.0969P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1785
_reflns_number_gt                1962
_reflns_number_total             3362
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja052108qsi20050426_035021.cif
_cod_data_source_block           ni2bptz2
_cod_database_code               4111916
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.45468(11) 0.22866(8) 0.70952(9) 0.0264(3) Uani 1 1 d . . .
Cl2 Cl 0.8248(2) 0.24359(18) 0.3837(2) 0.0400(6) Uani 1 1 d . . .
N7 N 0.2223(8) 0.1468(6) 0.6960(6) 0.0360(16) Uani 1 1 d . . .
N2 N 0.4738(7) 0.0838(5) 0.5863(5) 0.0281(15) Uani 1 1 d . . .
O5 O 0.6987(7) 0.1625(5) 0.2914(5) 0.0516(17) Uani 1 1 d . . .
N3 N 0.4718(7) 0.0302(5) 0.3914(5) 0.0289(15) Uani 1 1 d . . .
N4 N 0.6922(7) 0.3122(5) 0.7301(5) 0.0288(15) Uani 1 1 d . . .
N1 N 0.3816(7) 0.2996(5) 0.5619(5) 0.0288(15) Uani 1 1 d . . .
C6 C 0.4547(8) 0.1085(6) 0.4849(7) 0.0260(17) Uani 1 1 d . . .
N6 N 0.4255(7) 0.3900(6) 0.8096(5) 0.0299(15) Uani 1 1 d . . .
N5 N 0.5492(8) 0.1436(5) 0.8461(6) 0.0331(16) Uani 1 1 d . . .
O6 O 0.8433(8) 0.3674(5) 0.3614(6) 0.0607(19) Uani 1 1 d . . .
O7 O 0.7810(7) 0.2424(6) 0.4870(5) 0.0580(18) Uani 1 1 d . . .
C1 C 0.3246(9) 0.4060(7) 0.5486(7) 0.0335(19) Uani 1 1 d . . .
H1 H 0.3080 0.4558 0.6132 0.040 Uiso 1 1 calc R . .
C2 C 0.2880(9) 0.4487(7) 0.4472(7) 0.036(2) Uani 1 1 d . . .
H2 H 0.2495 0.5265 0.4429 0.043 Uiso 1 1 calc R . .
C5 C 0.3978(8) 0.2307(7) 0.4676(7) 0.0286(18) Uani 1 1 d . . .
C4 C 0.3642(9) 0.2658(7) 0.3624(7) 0.0348(19) Uani 1 1 d . . .
H4 H 0.3792 0.2147 0.2979 0.042 Uiso 1 1 calc R . .
C3 C 0.3076(9) 0.3789(7) 0.3550(7) 0.038(2) Uani 1 1 d . . .
H3 H 0.2827 0.4068 0.2842 0.045 Uiso 1 1 calc R . .
O8 O 0.9735(8) 0.1954(6) 0.3933(8) 0.085(3) Uani 1 1 d . . .
Cl1 Cl 0.1256(9) 0.2803(7) 0.0289(6) 0.0476(7) Uani 0.47 1 d PD A -1
O11 O 0.1384(18) 0.1974(11) 0.1086(9) 0.061(3) Uani 0.47 1 d PD A -1
O21 O 0.2082(18) 0.4039(11) 0.0836(14) 0.095(5) Uani 0.47 1 d PD A -1
O31 O -0.0384(10) 0.2873(11) -0.0239(10) 0.067(3) Uani 0.47 1 d PD A -1
O41 O 0.1976(14) 0.2340(11) -0.0566(10) 0.061(3) Uani 0.47 1 d PD A -1
Cl1B Cl 0.1374(8) 0.2807(6) 0.0346(6) 0.0476(7) Uani 0.53 1 d PD B -2
O12 O 0.2624(11) 0.2163(9) 0.0847(8) 0.061(3) Uani 0.53 1 d PD B -2
O22 O 0.0312(12) 0.2899(13) 0.1052(9) 0.095(5) Uani 0.53 1 d PD B -2
O32 O 0.0482(12) 0.2075(10) -0.0731(7) 0.067(3) Uani 0.53 1 d PD B -2
O42 O 0.2097(16) 0.4058(8) 0.0354(12) 0.061(3) Uani 0.53 1 d PD B -2
C13 C 0.0952(11) 0.1041(8) 0.6924(8) 0.046(2) Uani 1 1 d . . .
C7 C 0.8224(9) 0.3601(7) 0.7468(7) 0.0313(18) Uani 1 1 d . . .
C10 C 0.7170(11) 0.0632(8) 1.0205(8) 0.053(3) Uani 1 1 d . . .
H10A H 0.6780 0.0906 1.0864 0.080 Uiso 1 1 calc R . .
H10B H 0.8326 0.0982 1.0371 0.080 Uiso 1 1 calc R . .
H10C H 0.7020 -0.0293 1.0042 0.080 Uiso 1 1 calc R . .
C8 C 0.9894(9) 0.4227(8) 0.7666(9) 0.054(3) Uani 1 1 d . . .
H8C H 1.0177 0.4152 0.6943 0.082 Uiso 1 1 calc R . .
H8A H 1.0627 0.3826 0.8195 0.082 Uiso 1 1 calc R . .
H8B H 0.9999 0.5122 0.7993 0.082 Uiso 1 1 calc R . .
C11 C 0.4078(9) 0.4860(8) 0.8527(7) 0.0345(19) Uani 1 1 d . . .
C12 C 0.3812(11) 0.6074(7) 0.9043(8) 0.045(2) Uani 1 1 d . . .
H12C H 0.3080 0.6425 0.8470 0.068 Uiso 1 1 calc R . .
H12B H 0.4853 0.6653 0.9344 0.068 Uiso 1 1 calc R . .
H12A H 0.3325 0.5964 0.9665 0.068 Uiso 1 1 calc R . .
C9 C 0.6257(10) 0.1078(7) 0.9222(7) 0.036(2) Uani 1 1 d . . .
C14 C -0.0728(11) 0.0522(9) 0.6873(11) 0.086(4) Uani 1 1 d . . .
H14A H -0.1117 0.1092 0.7397 0.129 Uiso 1 1 calc R . .
H14B H -0.0763 -0.0310 0.7094 0.129 Uiso 1 1 calc R . .
H14C H -0.1423 0.0440 0.6096 0.129 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'
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'
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
N7 Ni1 N1 92.1(2) . .
N7 Ni1 N4 177.8(3) . .
N1 Ni1 N4 89.8(2) . .
N7 Ni1 N6 90.2(2) . .
N1 Ni1 N6 92.4(2) . .
N4 Ni1 N6 88.6(2) . .
N7 Ni1 N5 92.1(2) . .
N1 Ni1 N5 171.7(2) . .
N4 Ni1 N5 86.1(2) . .
N6 Ni1 N5 94.8(2) . .
N7 Ni1 N2 90.9(2) . .
N1 Ni1 N2 77.8(2) . .
N4 Ni1 N2 90.6(2) . .
N6 Ni1 N2 170.1(2) . .
N5 Ni1 N2 95.0(2) . .
O6 Cl2 O7 110.2(4) . .
O6 Cl2 O8 110.3(4) . .
O7 Cl2 O8 108.8(5) . .
O6 Cl2 O5 109.5(4) . .
O7 Cl2 O5 109.1(3) . .
O8 Cl2 O5 108.9(4) . .
C13 N7 Ni1 177.5(7) . .
C6 N2 N3 118.4(6) . 2_656
C6 N2 Ni1 116.1(5) . .
N3 N2 Ni1 124.9(5) 2_656 .
C6 N3 N2 115.1(6) . 2_656
C7 N4 Ni1 176.5(6) . .
C1 N1 C5 115.7(7) . .
C1 N1 Ni1 128.6(6) . .
C5 N1 Ni1 115.7(5) . .
N2 C6 N3 126.4(6) . .
N2 C6 C5 115.5(7) . .
N3 C6 C5 117.9(7) . .
C11 N6 Ni1 171.2(6) . .
C9 N5 Ni1 168.7(6) . .
N1 C1 C2 124.1(8) . .
N1 C1 H1 117.9 . .
C2 C1 H1 117.9 . .
C3 C2 C1 118.8(7) . .
C3 C2 H2 120.6 . .
C1 C2 H2 120.6 . .
N1 C5 C4 124.2(7) . .
N1 C5 C6 114.1(7) . .
C4 C5 C6 121.7(7) . .
C5 C4 C3 117.0(8) . .
C5 C4 H4 121.5 . .
C3 C4 H4 121.5 . .
C2 C3 C4 120.1(8) . .
C2 C3 H3 119.9 . .
C4 C3 H3 119.9 . .
O21 Cl1 O31 108.3(4) . .
O21 Cl1 O41 109.3(10) . .
O31 Cl1 O41 108.5(4) . .
O21 Cl1 O11 110.4(10) . .
O31 Cl1 O11 112.0(10) . .
O41 Cl1 O11 108.3(4) . .
O42 Cl1B O32 116.6(9) . .
O42 Cl1B O22 106.9(9) . .
O32 Cl1B O22 108.4(4) . .
O42 Cl1B O12 108.0(4) . .
O32 Cl1B O12 108.5(4) . .
O22 Cl1B O12 108.2(4) . .
N7 C13 C14 178.2(9) . .
N4 C7 C8 179.0(8) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C7 C8 H8C 109.5 . .
C7 C8 H8A 109.5 . .
H8C C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8C C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
N6 C11 C12 178.3(8) . .
C11 C12 H12C 109.5 . .
C11 C12 H12B 109.5 . .
H12C C12 H12B 109.5 . .
C11 C12 H12A 109.5 . .
H12C C12 H12A 109.5 . .
H12B C12 H12A 109.5 . .
N5 C9 C10 177.6(9) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N7 2.045(7) .
Ni1 N1 2.067(6) .
Ni1 N4 2.072(6) .
Ni1 N6 2.075(7) .
Ni1 N5 2.077(7) .
Ni1 N2 2.078(6) .
Cl2 O6 1.408(6) .
Cl2 O7 1.423(6) .
Cl2 O8 1.431(6) .
Cl2 O5 1.448(6) .
N7 C13 1.123(9) .
N2 C6 1.294(9) .
N2 N3 1.418(8) 2_656
N3 C6 1.384(9) .
N3 N2 1.418(8) 2_656
N4 C7 1.131(8) .
N1 C1 1.328(9) .
N1 C5 1.340(9) .
C6 C5 1.497(10) .
N6 C11 1.145(9) .
N5 C9 1.154(9) .
C1 C2 1.375(10) .
C1 H1 0.9500 .
C2 C3 1.335(10) .
C2 H2 0.9500 .
C5 C4 1.380(10) .
C4 C3 1.384(11) .
C4 H4 0.9500 .
C3 H3 0.9500 .
Cl1 O21 1.419(5) .
Cl1 O31 1.419(5) .
Cl1 O41 1.419(5) .
Cl1 O11 1.420(5) .
Cl1B O42 1.419(4) .
Cl1B O32 1.419(4) .
Cl1B O22 1.420(4) .
Cl1B O12 1.420(4) .
C13 C14 1.471(11) .
C7 C8 1.458(10) .
C10 C9 1.454(11) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C8 H8C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C11 C12 1.451(11) .
C12 H12C 0.9800 .
C12 H12B 0.9800 .
C12 H12A 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
