#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:13:47 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178890 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/19/4111917.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_4111917
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         '2(C16 H14 Mn N8), 4(B F4), 3(C2 H3 N)'
_chemical_formula_sum            'C38 H37 B4 F16 Mn2 N19'
_chemical_formula_weight         1216.99
_chemical_name_common            {[Mn(bptz)(CH3CN)2][BF4]2}%ψ1.5nCH3CN
_chemical_name_systematic
; 
 ? 
;
_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 28 2004'
_audit_creation_method
;
SHELXL-97, PLATON, and text editor.
;
_cell_angle_alpha                99.48(3)
_cell_angle_beta                 107.53(3)
_cell_angle_gamma                102.27(3)
_cell_formula_units_Z            1
_cell_length_a                   9.1350(18)
_cell_length_b                   10.859(2)
_cell_length_c                   14.631(3)
_cell_measurement_temperature    110(2)
_cell_volume                     1311.0(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0802
_diffrn_reflns_av_sigmaI/netI    0.1328
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12767
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.9168
_exptl_absorpt_correction_T_min  0.8431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       plate
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         4445
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0582P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                2315
_reflns_number_total             4445
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja052108qsi20050426_035055.cif
_cod_data_source_block           global
_cod_original_cell_volume        1311.0(5)
_cod_database_code               4111917
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
Mn1 Mn 0.00912(8) 0.28893(6) 0.67173(5) 0.0247(2) Uani 1 1 d . . .
B1 B 0.0752(7) 0.2324(5) 0.3510(4) 0.0284(13) Uani 1 1 d . . .
F2 F 0.2104(3) 0.3269(3) 0.4174(2) 0.0536(9) Uani 1 1 d . . .
F1 F 0.0892(3) 0.1117(2) 0.3604(2) 0.0465(8) Uani 1 1 d . . .
F4 F -0.0563(3) 0.2531(3) 0.3746(2) 0.0548(9) Uani 1 1 d . . .
F3 F 0.0585(4) 0.2447(3) 0.2575(2) 0.0656(10) Uani 1 1 d . . .
N4 N -0.2385(4) 0.1837(3) 0.5698(3) 0.0258(9) Uani 1 1 d . . .
N3 N -0.1436(4) 0.4314(3) 0.5006(3) 0.0245(9) Uani 1 1 d . . .
N6 N 0.1457(4) 0.0681(3) 0.5710(3) 0.0207(9) Uani 1 1 d . . .
N5 N 0.0181(4) 0.1132(3) 0.5623(2) 0.0196(9) Uani 1 1 d . . .
N2 N -0.0085(4) 0.4208(3) 0.5617(3) 0.0264(9) Uani 1 1 d . . .
N7 N -0.0329(5) 0.4418(4) 0.7674(3) 0.0360(11) Uani 1 1 d . . .
N8 N 0.0757(4) 0.1878(4) 0.7849(3) 0.0341(10) Uani 1 1 d . . .
N1 N 0.2556(4) 0.3893(3) 0.6822(3) 0.0219(9) Uani 1 1 d . . .
C5 C 0.2771(5) 0.4741(4) 0.6272(3) 0.0216(11) Uani 1 1 d . . .
C12 C -0.1218(5) 0.0433(4) 0.4916(3) 0.0176(10) Uani 1 1 d . . .
C11 C -0.2600(5) 0.0961(4) 0.4882(3) 0.0204(10) Uani 1 1 d . . .
C10 C -0.3994(5) 0.0538(4) 0.4070(3) 0.0276(11) Uani 1 1 d . . .
H10 H -0.4095 -0.0086 0.3501 0.033 Uiso 1 1 calc R . .
C9 C -0.5243(5) 0.1054(4) 0.4114(4) 0.0307(12) Uani 1 1 d . . .
H9 H -0.6213 0.0806 0.3564 0.037 Uiso 1 1 calc R . .
C6 C 0.1302(5) 0.4902(4) 0.5595(3) 0.0216(11) Uani 1 1 d . . .
C3 C 0.5591(5) 0.5214(4) 0.6961(3) 0.0301(12) Uani 1 1 d . . .
H3 H 0.6635 0.5677 0.7021 0.036 Uiso 1 1 calc R . .
C1 C 0.3862(5) 0.3687(4) 0.7432(3) 0.0290(12) Uani 1 1 d . . .
H1 H 0.3726 0.3075 0.7815 0.035 Uiso 1 1 calc R . .
C7 C -0.3624(5) 0.2313(4) 0.5734(4) 0.0344(13) Uani 1 1 d . . .
H7 H -0.3500 0.2933 0.6311 0.041 Uiso 1 1 calc R . .
C4 C 0.4270(5) 0.5422(4) 0.6314(3) 0.0298(12) Uani 1 1 d . . .
H4 H 0.4381 0.6011 0.5909 0.036 Uiso 1 1 calc R . .
C8 C -0.5061(5) 0.1926(4) 0.4959(4) 0.0348(13) Uani 1 1 d . . .
H8 H -0.5921 0.2261 0.5010 0.042 Uiso 1 1 calc R . .
C2 C 0.5391(5) 0.4331(4) 0.7522(3) 0.0260(11) Uani 1 1 d . . .
H2 H 0.6291 0.4170 0.7963 0.031 Uiso 1 1 calc R . .
C13 C -0.0362(5) 0.5198(5) 0.8298(4) 0.0316(12) Uani 1 1 d . . .
C14 C -0.0436(6) 0.6164(5) 0.9088(3) 0.0410(14) Uani 1 1 d . . .
H14A H -0.1114 0.6692 0.8801 0.062 Uiso 1 1 calc R . .
H14B H 0.0643 0.6726 0.9477 0.062 Uiso 1 1 calc R . .
H14C H -0.0887 0.5725 0.9516 0.062 Uiso 1 1 calc R . .
C15 C 0.0684(6) 0.1189(5) 0.8355(4) 0.0340(13) Uani 1 1 d . . .
C16 C 0.0547(8) 0.0328(6) 0.8990(4) 0.0679(19) Uani 1 1 d . . .
H16C H -0.0445 0.0283 0.9129 0.102 Uiso 1 1 calc R . .
H16A H 0.1462 0.0655 0.9610 0.102 Uiso 1 1 calc R . .
H16B H 0.0529 -0.0541 0.8663 0.102 Uiso 1 1 calc R . .
C18 C 0.3902(8) 0.8403(8) 0.8582(5) 0.096(3) Uani 1 1 d . . .
H18B H 0.3515 0.8458 0.9139 0.144 Uiso 1 1 calc R . .
H18C H 0.3060 0.7811 0.7990 0.144 Uiso 1 1 calc R . .
H18A H 0.4188 0.9268 0.8461 0.144 Uiso 1 1 calc R . .
N9 N 0.6411(9) 0.7548(7) 0.8993(7) 0.155(4) Uani 1 1 d . . .
C17 C 0.5312(10) 0.7913(8) 0.8815(6) 0.101(3) Uani 1 1 d . . .
F7 F 0.2572(13) 0.8780(9) 1.0610(6) 0.0635(15) Uani 0.59 1 d PD A -1
F5 F 0.4823(8) 0.8367(10) 1.1498(8) 0.0797(16) Uani 0.59 1 d PD A -1
B2 B 0.3207(10) 0.8154(8) 1.1311(6) 0.046(2) Uani 0.59 1 d PD A -1
F6 F 0.2423(7) 0.6833(5) 1.0970(5) 0.0627(19) Uani 0.59 1 d PD A -1
F8 F 0.2974(8) 0.8590(6) 1.2171(5) 0.083(2) Uani 0.59 1 d PD A -1
B2B B 0.3227(13) 0.8549(10) 1.1405(8) 0.046(2) Uani 0.41 1 d PD B -2
F5B F 0.4800(12) 0.8537(15) 1.1665(12) 0.0797(16) Uani 0.41 1 d PD B -2
F6B F 0.2273(11) 0.7368(8) 1.1396(7) 0.0627(19) Uani 0.41 1 d PD B -2
F7B F 0.2707(19) 0.8772(13) 1.0476(8) 0.0635(15) Uani 0.41 1 d PD B -2
F8B F 0.3086(12) 0.9512(8) 1.2078(7) 0.083(2) Uani 0.41 1 d PD B -2
C2S C 0.4253(10) 0.501(3) 0.988(2) 0.084(3) Uani 0.50 1 d PD C -3
N1S N 0.2950(10) 0.4982(13) 0.9599(9) 0.095(4) Uani 0.50 1 d PD C -3
C3S C 0.5907(12) 0.499(4) 1.023(3) 0.084(3) Uani 0.50 1 d PD C -3
H3S1 H 0.5962 0.4117 1.0294 0.126 Uiso 0.50 1 calc P D -3
H3S2 H 0.6476 0.5614 1.0872 0.126 Uiso 0.50 1 calc P E -3
H3S3 H 0.6405 0.5233 0.9752 0.126 Uiso 0.50 1 calc P F -3
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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
N8 Mn1 N7 93.81(14) . .
N8 Mn1 N4 108.67(14) . .
N7 Mn1 N4 101.46(14) . .
N8 Mn1 N1 97.32(14) . .
N7 Mn1 N1 99.20(14) . .
N4 Mn1 N1 145.35(13) . .
N8 Mn1 N5 87.18(13) . .
N7 Mn1 N5 172.45(14) . .
N4 Mn1 N5 71.18(13) . .
N1 Mn1 N5 88.09(12) . .
N8 Mn1 N2 168.41(14) . .
N7 Mn1 N2 85.99(14) . .
N4 Mn1 N2 82.68(13) . .
N1 Mn1 N2 71.32(13) . .
N5 Mn1 N2 94.54(12) . .
F3 B1 F1 111.0(4) . .
F3 B1 F2 109.1(4) . .
F1 B1 F2 109.6(4) . .
F3 B1 F4 110.1(4) . .
F1 B1 F4 109.4(4) . .
F2 B1 F4 107.5(4) . .
C11 N4 C7 117.6(4) . .
C11 N4 Mn1 119.2(3) . .
C7 N4 Mn1 120.6(3) . .
N2 N3 C6 116.9(3) . 2_566
C12 N6 N5 116.1(3) 2_556 .
N6 N5 C12 118.2(3) . .
N6 N5 Mn1 125.0(3) . .
C12 N5 Mn1 116.3(3) . .
N3 N2 C6 118.2(4) . .
N3 N2 Mn1 125.3(3) . .
C6 N2 Mn1 116.5(3) . .
C13 N7 Mn1 169.2(4) . .
C15 N8 Mn1 161.7(4) . .
C5 N1 C1 117.9(4) . .
C5 N1 Mn1 120.0(3) . .
C1 N1 Mn1 122.2(3) . .
N1 C5 C4 123.2(4) . .
N1 C5 C6 115.7(4) . .
C4 C5 C6 121.1(4) . .
N6 C12 N5 125.7(4) 2_556 .
N6 C12 C11 118.8(4) 2_556 .
N5 C12 C11 115.5(4) . .
N4 C11 C10 123.9(4) . .
N4 C11 C12 114.5(4) . .
C10 C11 C12 121.6(4) . .
C11 C10 C9 117.7(4) . .
C11 C10 H10 121.2 . .
C9 C10 H10 121.1 . .
C8 C9 C10 119.2(4) . .
C8 C9 H9 120.4 . .
C10 C9 H9 120.4 . .
N3 C6 N2 124.9(4) 2_566 .
N3 C6 C5 118.6(4) 2_566 .
N2 C6 C5 116.5(4) . .
C2 C3 C4 119.8(4) . .
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
N1 C1 C2 122.5(4) . .
N1 C1 H1 118.7 . .
C2 C1 H1 118.7 . .
N4 C7 C8 122.0(5) . .
N4 C7 H7 119.0 . .
C8 C7 H7 119.0 . .
C3 C4 C5 117.7(4) . .
C3 C4 H4 121.1 . .
C5 C4 H4 121.1 . .
C9 C8 C7 119.6(4) . .
C9 C8 H8 120.2 . .
C7 C8 H8 120.2 . .
C3 C2 C1 118.9(4) . .
C3 C2 H2 120.6 . .
C1 C2 H2 120.6 . .
N7 C13 C14 178.7(5) . .
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 . .
N8 C15 C16 178.3(6) . .
C15 C16 H16C 109.5 . .
C15 C16 H16A 109.5 . .
H16C C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16C C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C17 C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C17 C18 H18A 109.5 . .
H18B C18 H18A 109.5 . .
H18C C18 H18A 109.5 . .
N9 C17 C18 179.1(11) . .
F8 B2 F7 110.7(7) . .
F8 B2 F5 108.9(7) . .
F7 B2 F5 110.1(7) . .
F8 B2 F6 107.5(7) . .
F7 B2 F6 108.8(7) . .
F5 B2 F6 110.7(7) . .
F8B B2B F5B 109.2(9) . .
F8B B2B F7B 109.5(9) . .
F5B B2B F7B 110.2(9) . .
F8B B2B F6B 109.0(8) . .
F5B B2B F6B 110.4(9) . .
F7B B2B F6B 108.6(8) . .
N1S C2S C3S 178(2) . .
C2S C3S H3S1 109.5 . .
C2S C3S H3S2 109.5 . .
H3S1 C3S H3S2 109.4 . .
C2S C3S H3S3 109.5 . .
H3S1 C3S H3S3 109.5 . .
H3S2 C3S H3S3 109.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N8 2.143(4) .
Mn1 N7 2.166(4) .
Mn1 N4 2.225(4) .
Mn1 N1 2.231(4) .
Mn1 N5 2.313(4) .
Mn1 N2 2.318(4) .
B1 F3 1.363(6) .
B1 F1 1.369(6) .
B1 F2 1.390(6) .
B1 F4 1.397(6) .
N4 C11 1.333(5) .
N4 C7 1.351(5) .
N3 N2 1.328(5) .
N3 C6 1.335(5) 2_566
N6 C12 1.324(5) 2_556
N6 N5 1.337(4) .
N5 C12 1.346(5) .
N2 C6 1.341(5) .
N7 C13 1.151(6) .
N8 C15 1.141(5) .
N1 C5 1.340(5) .
N1 C1 1.344(5) .
C5 C4 1.389(6) .
C5 C6 1.473(6) .
C12 N6 1.324(5) 2_556
C12 C11 1.484(6) .
C11 C10 1.380(6) .
C10 C9 1.388(6) .
C10 H10 0.9500 .
C9 C8 1.369(6) .
C9 H9 0.9500 .
C6 N3 1.335(5) 2_566
C3 C2 1.378(6) .
C3 C4 1.380(6) .
C3 H3 0.9500 .
C1 C2 1.379(6) .
C1 H1 0.9500 .
C7 C8 1.378(6) .
C7 H7 0.9500 .
C4 H4 0.9500 .
C8 H8 0.9500 .
C2 H2 0.9500 .
C13 C14 1.455(6) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C16 1.435(7) .
C16 H16C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C18 C17 1.465(11) .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C18 H18A 0.9800 .
N9 C17 1.131(10) .
F7 B2 1.375(8) .
F5 B2 1.378(8) .
B2 F8 1.365(8) .
B2 F6 1.390(8) .
B2B F8B 1.369(9) .
B2B F5B 1.375(9) .
B2B F7B 1.378(9) .
B2B F6B 1.385(9) .
C2S N1S 1.129(4) .
C2S C3S 1.447(4) .
C3S H3S1 0.9797 .
C3S H3S2 0.9807 .
C3S H3S3 0.9796 .
