#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:40:04 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180150 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/47/7104745.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_7104745
loop_
_publ_author_name
'Duriska, Martin B'
'Neville, Suzanne M'
'Batten, Stuart R'
_publ_section_title
;
 Variable length ligands: a new class of bridging ligands for
 supramolecular chemistry and crystal engineering.
;
_journal_issue                   37
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5579
_journal_page_last               5581
_journal_paper_doi               10.1039/b910994c
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety
;
C54 H76 Ba2 Fe N14 O10 S6, 2(C H Cl3)
;
_chemical_formula_sum            'C56 H78 Ba2 Cl6 Fe N14 O10 S6'
_chemical_formula_weight         1842.91
_chemical_name_systematic
;
?
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '9 November 2005'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.6672(13)
_cell_length_b                   14.4533(5)
_cell_length_c                   17.3796(6)
_cell_measurement_reflns_used    111
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.71
_cell_measurement_theta_min      2.66
_cell_volume                     7703.4(5)
_computing_cell_refinement       'SMART (BrukerAXS, 1997)'
_computing_data_collection       'SMART (BrukerAXS, 1997)'
_computing_data_reduction        'SAINT+ (BrukerAXS, 1997)'
_computing_molecular_graphics    'MERCURY 1.4 (Bruno et al., 2002)'
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'
_computing_structure_refinement  X-SEED
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'APEX X8'
_diffrn_measurement_method       'scans in phi and omega'
_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  0.0814
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            68351
_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_T_max  0.7923
_exptl_absorpt_correction_T_min  0.7367
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3712
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.775
_refine_diff_density_min         -1.575
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         6000
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0966
_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)+(0.0683P)²+156.9579P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2112
_refine_ls_wR_factor_ref         0.2308
_reflns_number_gt                4595
_reflns_number_total             6000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910994c.txt
_cod_data_source_block           E
_cod_original_sg_symbol_H-M      Cmca
_cod_database_code               7104745
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x, -y, -z'
'-x, y+1/2, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x, y, z'
'x, -y-1/2, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba1 Ba 0.2500 0.32468(4) 0.2500 0.02873(18) Uani 1 2 d S . .
Fe1 Fe 0.0000 0.0000 0.5000 0.0247(4) Uani 1 4 d S . .
S1 S 0.13781(6) 0.13793(15) 0.11574(12) 0.0399(5) Uani 1 1 d . . .
O1 O 0.17691(18) 0.3824(3) 0.1693(3) 0.0373(12) Uani 1 1 d . . .
N1 N 0.2247(2) 0.1725(4) 0.1519(4) 0.0324(13) Uani 1 1 d . . .
C1 C 0.1290(3) 0.3344(5) 0.2690(5) 0.0390(18) Uani 1 1 d . . .
H1A H 0.1024 0.3516 0.2981 0.047 Uiso 1 1 calc R . .
H1B H 0.1223 0.2781 0.2388 0.047 Uiso 1 1 calc R . .
H3 H 0.257(3) 0.562(4) 0.215(4) 0.047 Uiso 1 1 d D . .
S2A S 0.0000 0.2270(4) 0.7067(3) 0.113(2) Uani 1 2 d S A 1
O2 O 0.26044(18) 0.3978(4) 0.1029(3) 0.0366(12) Uani 1 1 d . . .
N2 N 0.1644(2) 0.3138(4) 0.3236(4) 0.0341(14) Uani 1 1 d . . .
C2 C 0.1406(3) 0.4129(6) 0.2140(6) 0.046(2) Uani 1 1 d . . .
H2A H 0.1156 0.4273 0.1801 0.055 Uiso 1 1 calc R . .
H2B H 0.1484 0.4693 0.2433 0.055 Uiso 1 1 calc R . .
O3 O 0.2500 0.5138(5) 0.2500 0.054(2) Uani 1 2 d SD . .
N3 N 0.05172(18) 0.0864(4) 0.4456(4) 0.0304(12) Uani 1 1 d . . .
C3 C 0.1849(3) 0.4381(5) 0.1035(5) 0.0403(19) Uani 1 1 d . . .
H3A H 0.1937 0.5012 0.1192 0.048 Uiso 1 1 calc R . .
H3B H 0.1582 0.4428 0.0716 0.048 Uiso 1 1 calc R . .
N4 N 0.0000 0.0895(6) 0.5953(6) 0.035(2) Uani 1 2 d S A .
C4 C 0.2210(3) 0.3926(6) 0.0582(5) 0.0425(19) Uani 1 1 d . . .
H4A H 0.2136 0.3272 0.0478 0.051 Uiso 1 1 calc R . .
H4B H 0.2250 0.4247 0.0084 0.051 Uiso 1 1 calc R . .
C5 C 0.2984(3) 0.3721(6) 0.0594(5) 0.043(2) Uani 1 1 d . . .
H5A H 0.3019 0.4146 0.0151 0.051 Uiso 1 1 calc R . .
H5B H 0.2948 0.3085 0.0392 0.051 Uiso 1 1 calc R . .
C6 C 0.3376(3) 0.3766(6) 0.1088(5) 0.045(2) Uani 1 1 d . . .
H6A H 0.3413 0.4409 0.1272 0.054 Uiso 1 1 calc R . .
H6B H 0.3635 0.3605 0.0776 0.054 Uiso 1 1 calc R . .
C7 C 0.1651(2) 0.2146(5) 0.3435(4) 0.0293(14) Uani 1 1 d . . .
H7A H 0.1895 0.2039 0.3798 0.035 Uiso 1 1 calc R . .
H7B H 0.1715 0.1790 0.2962 0.035 Uiso 1 1 calc R . .
C8 C 0.1238(2) 0.1755(5) 0.3792(4) 0.0272(14) Uani 1 1 d . . .
C9 C 0.1157(2) 0.1797(5) 0.4577(4) 0.0340(16) Uani 1 1 d . . .
H9 H 0.1349 0.2129 0.4907 0.041 Uiso 1 1 calc R . .
C10 C 0.0797(2) 0.1351(5) 0.4875(4) 0.0326(15) Uani 1 1 d . . .
H10 H 0.0745 0.1395 0.5413 0.039 Uiso 1 1 calc R . .
C11 C 0.0585(2) 0.0850(5) 0.3687(4) 0.0320(15) Uani 1 1 d . . .
H11 H 0.0385 0.0524 0.3370 0.038 Uiso 1 1 calc R . .
C12 C 0.0935(2) 0.1290(5) 0.3344(4) 0.0304(14) Uani 1 1 d . . .
H12 H 0.0967 0.1273 0.2801 0.036 Uiso 1 1 calc R . .
C13 C 0.1885(2) 0.1583(4) 0.1372(4) 0.0277(14) Uani 1 1 d . . .
C14 C 0.0000 0.1463(9) 0.6419(7) 0.040(2) Uani 1 2 d S . .
Cl1 Cl 0.04548(18) 0.4945(6) 0.3694(7) 0.278(6) Uani 1 1 d . . .
Cl2 Cl 0.0000 0.3468(11) 0.4439(10) 0.315(11) Uani 1 2 d S . .
C15 C 0.0000 0.436(4) 0.367(3) 0.29(4) Uani 1 2 d S . .
H15 H 0.0000 0.4016 0.3172 0.349 Uiso 1 2 calc SR . .
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'
S S 0.1246 0.1234 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 '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
O3 Ba1 O1 72.48(11) . . ?
O3 Ba1 O1 72.48(11) . 8_545 ?
O1 Ba1 O1 145.0(2) . 8_545 ?
O3 Ba1 O2 67.69(11) . . ?
O1 Ba1 O2 60.95(16) . . ?
O1 Ba1 O2 104.89(16) 8_545 . ?
O3 Ba1 O2 67.69(11) . 8_545 ?
O1 Ba1 O2 104.89(16) . 8_545 ?
O1 Ba1 O2 60.95(16) 8_545 8_545 ?
O2 Ba1 O2 135.4(2) . 8_545 ?
O3 Ba1 N1 139.59(12) . 8_545 ?
O1 Ba1 N1 138.15(16) . 8_545 ?
O1 Ba1 N1 73.35(16) 8_545 8_545 ?
O2 Ba1 N1 143.10(16) . 8_545 ?
O2 Ba1 N1 77.20(16) 8_545 8_545 ?
O3 Ba1 N1 139.59(12) . . ?
O1 Ba1 N1 73.35(16) . . ?
O1 Ba1 N1 138.15(16) 8_545 . ?
O2 Ba1 N1 77.20(16) . . ?
O2 Ba1 N1 143.10(16) 8_545 . ?
N1 Ba1 N1 80.8(2) 8_545 . ?
O3 Ba1 N2 93.08(11) . . ?
O1 Ba1 N2 60.76(17) . . ?
O1 Ba1 N2 121.38(17) 8_545 . ?
O2 Ba1 N2 121.67(18) . . ?
O2 Ba1 N2 61.04(17) 8_545 . ?
N1 Ba1 N2 86.70(18) 8_545 . ?
N1 Ba1 N2 88.61(18) . . ?
O3 Ba1 N2 93.08(11) . 8_545 ?
O1 Ba1 N2 121.38(17) . 8_545 ?
O1 Ba1 N2 60.76(17) 8_545 8_545 ?
O2 Ba1 N2 61.04(17) . 8_545 ?
O2 Ba1 N2 121.67(18) 8_545 8_545 ?
N1 Ba1 N2 88.61(18) 8_545 8_545 ?
N1 Ba1 N2 86.70(18) . 8_545 ?
N2 Ba1 N2 173.8(2) . 8_545 ?
N4 Fe1 N4 180.000(1) . 9_556 ?
N4 Fe1 N3 90.6(2) . 9_556 ?
N4 Fe1 N3 89.4(2) 9_556 9_556 ?
N4 Fe1 N3 89.4(2) . 11 ?
N4 Fe1 N3 90.6(2) 9_556 11 ?
N3 Fe1 N3 89.3(3) 9_556 11 ?
N4 Fe1 N3 90.6(2) . 3_556 ?
N4 Fe1 N3 89.4(2) 9_556 3_556 ?
N3 Fe1 N3 90.7(3) 9_556 3_556 ?
N3 Fe1 N3 180.0(3) 11 3_556 ?
N4 Fe1 N3 89.4(2) . . ?
N4 Fe1 N3 90.6(2) 9_556 . ?
N3 Fe1 N3 179.999(1) 9_556 . ?
N3 Fe1 N3 90.7(3) 11 . ?
N3 Fe1 N3 89.3(3) 3_556 . ?
C3 O1 C2 113.5(6) . . ?
C3 O1 Ba1 116.0(5) . . ?
C2 O1 Ba1 116.6(5) . . ?
C13 N1 Ba1 121.5(5) . . ?
N2 C1 C2 112.4(7) . . ?
N2 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
N2 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.9 . . ?
C5 O2 C4 112.6(6) . . ?
C5 O2 Ba1 118.5(4) . . ?
C4 O2 Ba1 112.3(4) . . ?
C1 N2 C7 111.0(6) . . ?
C1 N2 C6 110.8(6) . 8_545 ?
C7 N2 C6 114.1(6) . 8_545 ?
C1 N2 Ba1 111.7(4) . . ?
C7 N2 Ba1 98.2(4) . . ?
C6 N2 Ba1 110.5(4) 8_545 . ?
O1 C2 C1 107.1(6) . . ?
O1 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
O1 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.5 . . ?
Ba1 O3 H3 137(5) . . ?
C10 N3 C11 116.8(6) . . ?
C10 N3 Fe1 121.5(5) . . ?
C11 N3 Fe1 121.4(5) . . ?
O1 C3 C4 107.4(6) . . ?
O1 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 . . ?
O1 C3 H3B 110.2 . . ?
C4 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
C14 N4 Fe1 172.6(9) . . ?
O2 C4 C3 108.2(7) . . ?
O2 C4 H4A 110.1 . . ?
C3 C4 H4A 110.1 . . ?
O2 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
O2 C5 C6 110.0(6) . . ?
O2 C5 H5A 109.7 . . ?
C6 C5 H5A 109.7 . . ?
O2 C5 H5B 109.7 . . ?
C6 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
C5 C6 N2 113.5(7) . 8_545 ?
C5 C6 H6A 108.9 . . ?
N2 C6 H6A 108.9 8_545 . ?
C5 C6 H6B 108.9 . . ?
N2 C6 H6B 108.9 8_545 . ?
H6A C6 H6B 107.7 . . ?
N2 C7 C8 116.5(6) . . ?
N2 C7 H7A 108.2 . . ?
C8 C7 H7A 108.2 . . ?
N2 C7 H7B 108.2 . . ?
C8 C7 H7B 108.2 . . ?
H7A C7 H7B 107.3 . . ?
C9 C8 C12 116.9(6) . . ?
C9 C8 C7 122.3(7) . . ?
C12 C8 C7 120.7(6) . . ?
C10 C9 C8 119.4(7) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
N3 C10 C9 124.0(7) . . ?
N3 C10 H10 118.0 . . ?
C9 C10 H10 118.0 . . ?
N3 C11 C12 122.6(7) . . ?
N3 C11 H11 118.7 . . ?
C12 C11 H11 118.7 . . ?
C11 C12 C8 120.1(7) . . ?
C11 C12 H12 120.0 . . ?
C8 C12 H12 120.0 . . ?
N1 C13 S1 179.4(7) . . ?
N4 C14 S2A 179.4(12) . . ?
Cl1 C15 Cl1 117(4) . 11 ?
Cl1 C15 Cl2 110(2) . . ?
Cl1 C15 Cl2 110(2) 11 . ?
Cl1 C15 H15 106.2 . . ?
Cl1 C15 H15 106.2 11 . ?
Cl2 C15 H15 106.1 . . ?
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
Ba1 O3 2.734(8) . ?
Ba1 O1 2.772(6) . ?
Ba1 O1 2.773(6) 8_545 ?
Ba1 O2 2.785(5) . ?
Ba1 O2 2.785(5) 8_545 ?
Ba1 N1 2.889(6) 8_545 ?
Ba1 N1 2.890(6) . ?
Ba1 N2 2.923(6) . ?
Ba1 N2 2.923(6) 8_545 ?
Fe1 N4 2.101(10) . ?
Fe1 N4 2.101(10) 9_556 ?
Fe1 N3 2.229(6) 9_556 ?
Fe1 N3 2.229(6) 11 ?
Fe1 N3 2.229(6) 3_556 ?
Fe1 N3 2.229(6) . ?
S1 C13 1.627(8) . ?
O1 C3 1.421(9) . ?
O1 C2 1.426(9) . ?
N1 C13 1.155(9) . ?
C1 N2 1.474(11) . ?
C1 C2 1.525(11) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
S2A C14 1.622(13) . ?
O2 C5 1.437(9) . ?
O2 C4 1.438(10) . ?
N2 C7 1.475(9) . ?
N2 C6 1.486(10) 8_545 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O3 H3 0.95(7) . ?
N3 C10 1.327(9) . ?
N3 C11 1.353(9) . ?
C3 C4 1.509(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N4 C14 1.153(15) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.478(13) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N2 1.486(10) 8_545 ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.519(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.389(10) . ?
C8 C12 1.387(10) . ?
C9 C10 1.381(9) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.380(9) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
Cl1 C15 1.63(3) . ?
Cl2 C15 1.86(6) . ?
C15 Cl1 1.63(3) 11 ?
C15 H15 1.0000 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 N1 0.95(7) 2.02(6) 2.961(8) 173(8) 15
