#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/05/7010572.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_7010572
loop_
_publ_author_name
'Beer, Paul D.'
'Bernhardt, Paul V.'
_publ_section_title
;
 A ferrocene functionalised macrocyclic receptor for cations and anions
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1428
_journal_paper_doi               10.1039/b100439p
_journal_year                    2001
_chemical_formula_sum            'C34 H56 Cl2 Fe2 N6 O2'
_chemical_formula_weight         763.45
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.55(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.967(5)
_cell_length_b                   7.4043(8)
_cell_length_c                   33.060(10)
_cell_measurement_temperature    569(2)
_cell_volume                     3663.5(17)
_computing_cell_refinement       'SET4 in CAD4'
_computing_data_collection       CAD4
_computing_data_reduction        XCAD4
_computing_molecular_graphics    PLATON
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      569(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'ω-2θ 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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            3337
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        'less than 5%'
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  0.6409
_exptl_absorpt_correction_T_min  0.5919
_exptl_absorpt_correction_type   \y-scans
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0386
_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)+(0.0645P)²+5.5712P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                2509
_reflns_number_total             3204
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100439p.txt
_cod_data_source_block           pb66076
_cod_database_code               7010572
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.36840(3) 0.34625(6) 0.196015(13) 0.03904(17) Uani 1 1 d . . .
C1A C 0.4650(2) 0.4138(4) 0.15499(9) 0.0422(7) Uani 1 1 d . . .
C2A C 0.3792(2) 0.4634(4) 0.14027(10) 0.0482(8) Uani 1 1 d . . .
H2A H 0.3525 0.4233 0.1164 0.058 Uiso 1 1 calc R . .
C3A C 0.3414(3) 0.5857(5) 0.16856(12) 0.0571(9) Uani 1 1 d . . .
H3A H 0.2854 0.6393 0.1663 0.069 Uiso 1 1 calc R . .
C4A C 0.4028(3) 0.6120(4) 0.20051(11) 0.0550(9) Uani 1 1 d . . .
H4A H 0.3945 0.6856 0.2230 0.066 Uiso 1 1 calc R . .
C5A C 0.4792(2) 0.5069(4) 0.19242(10) 0.0482(8) Uani 1 1 d . . .
H5A H 0.5301 0.4993 0.2087 0.058 Uiso 1 1 calc R . .
C1B C 0.3802(2) 0.1718(5) 0.24397(10) 0.0511(8) Uani 1 1 d . . .
H1B H 0.4273 0.1660 0.2625 0.061 Uiso 1 1 calc R . .
C2B C 0.3738(3) 0.0769(5) 0.20714(12) 0.0605(10) Uani 1 1 d . . .
H2B H 0.4162 -0.0022 0.1969 0.073 Uiso 1 1 calc R . .
C3B C 0.2924(3) 0.1221(6) 0.18860(11) 0.0683(12) Uani 1 1 d . . .
H3B H 0.2712 0.0784 0.1640 0.082 Uiso 1 1 calc R . .
C4B C 0.2483(2) 0.2461(6) 0.21399(12) 0.0620(10) Uani 1 1 d . . .
H4B H 0.1927 0.2981 0.2091 0.074 Uiso 1 1 calc R . .
C5B C 0.3027(2) 0.2766(5) 0.24768(10) 0.0510(8) Uani 1 1 d . . .
H5B H 0.2898 0.3537 0.2691 0.061 Uiso 1 1 calc R . .
N1 N 0.57571(14) 0.1320(3) 0.03807(7) 0.0363(5) Uani 1 1 d . . .
H1A H 0.5397 0.2232 0.0455 0.044 Uiso 1 1 d R . .
N2 N 0.43778(15) -0.1075(3) 0.05129(7) 0.0381(6) Uani 1 1 d . . .
H2C H 0.4733 -0.0447 0.0346 0.046 Uiso 1 1 calc R . .
H2D H 0.3933 -0.0338 0.0590 0.046 Uiso 1 1 calc R . .
N3 N 0.48986(16) 0.1413(3) 0.11475(7) 0.0388(6) Uani 1 1 d . . .
H3C H 0.4453 0.1000 0.1303 0.047 Uiso 1 1 d R . .
C1 C 0.6432(2) 0.2002(5) 0.01030(10) 0.0453(8) Uani 1 1 d . . .
H1D H 0.6861 0.1055 0.0048 0.054 Uiso 1 1 calc R . .
H1E H 0.6749 0.3000 0.0229 0.054 Uiso 1 1 calc R . .
C2 C 0.61752(19) 0.0530(4) 0.07401(9) 0.0408(7) Uani 1 1 d . . .
H2E H 0.6565 0.1418 0.0866 0.049 Uiso 1 1 calc R . .
H2F H 0.6540 -0.0490 0.0660 0.049 Uiso 1 1 calc R . .
C3 C 0.54843(19) -0.0105(4) 0.10491(9) 0.0390(7) Uani 1 1 d . . .
C4 C 0.4902(2) -0.1616(4) 0.08741(9) 0.0435(7) Uani 1 1 d . . .
H4C H 0.5283 -0.2626 0.0803 0.052 Uiso 1 1 calc R . .
H4D H 0.4495 -0.2026 0.1081 0.052 Uiso 1 1 calc R . .
C5 C 0.3988(2) -0.2626(4) 0.02873(9) 0.0467(8) Uani 1 1 d . . .
H5C H 0.3540 -0.3211 0.0452 0.056 Uiso 1 1 calc R . .
H5D H 0.4452 -0.3501 0.0231 0.056 Uiso 1 1 calc R . .
C6 C 0.5982(2) -0.0949(5) 0.14101(10) 0.0568(9) Uani 1 1 d . . .
H6A H 0.6357 -0.0056 0.1536 0.085 Uiso 1 1 calc R . .
H6B H 0.6342 -0.1937 0.1318 0.085 Uiso 1 1 calc R . .
H6C H 0.5557 -0.1384 0.1603 0.085 Uiso 1 1 calc R . .
C7 C 0.5323(2) 0.2940(5) 0.13539(10) 0.0481(8) Uani 1 1 d . . .
H7A H 0.5662 0.3637 0.1160 0.058 Uiso 1 1 calc R . .
H7B H 0.5736 0.2490 0.1558 0.058 Uiso 1 1 calc R . .
Cl1 Cl 0.25364(6) 0.08623(17) 0.07172(3) 0.0742(3) Uani 1 1 d . . .
O1 O 0.1213(2) 0.1951(4) -0.00426(11) 0.0924(10) Uani 1 1 d . . .
H1 H 0.1517 0.1681 0.0145 0.111 Uiso 1 1 d R . .
H2 H 0.1525 0.1964 -0.0261 0.111 Uiso 1 1 d 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'
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'
Fe Fe 0.3463 0.8444 '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
C3B Fe1 C2B 40.34(17) . . ?
C3B Fe1 C3A 123.53(18) . . ?
C2B Fe1 C3A 161.15(17) . . ?
C3B Fe1 C4B 40.66(17) . . ?
C2B Fe1 C4B 67.85(16) . . ?
C3A Fe1 C4B 106.02(15) . . ?
C3B Fe1 C4A 160.16(18) . . ?
C2B Fe1 C4A 157.77(18) . . ?
C3A Fe1 C4A 40.44(15) . . ?
C4B Fe1 C4A 123.55(16) . . ?
C3B Fe1 C2A 106.73(15) . . ?
C2B Fe1 C2A 125.23(15) . . ?
C3A Fe1 C2A 40.88(14) . . ?
C4B Fe1 C2A 119.66(15) . . ?
C4A Fe1 C2A 68.53(15) . . ?
C3B Fe1 C5A 157.54(17) . . ?
C2B Fe1 C5A 123.47(15) . . ?
C3A Fe1 C5A 67.92(15) . . ?
C4B Fe1 C5A 161.16(16) . . ?
C4A Fe1 C5A 40.42(14) . . ?
C2A Fe1 C5A 68.25(14) . . ?
C3B Fe1 C5B 67.71(15) . . ?
C2B Fe1 C5B 67.63(14) . . ?
C3A Fe1 C5B 119.89(14) . . ?
C4B Fe1 C5B 39.87(15) . . ?
C4A Fe1 C5B 107.79(14) . . ?
C2A Fe1 C5B 154.51(14) . . ?
C5A Fe1 C5B 126.28(14) . . ?
C3B Fe1 C1B 67.76(16) . . ?
C2B Fe1 C1B 40.38(15) . . ?
C3A Fe1 C1B 155.58(15) . . ?
C4B Fe1 C1B 67.36(14) . . ?
C4A Fe1 C1B 122.12(16) . . ?
C2A Fe1 C1B 163.09(14) . . ?
C5A Fe1 C1B 110.33(15) . . ?
C5B Fe1 C1B 40.02(13) . . ?
C3B Fe1 C1A 121.18(15) . . ?
C2B Fe1 C1A 109.40(13) . . ?
C3A Fe1 C1A 68.31(14) . . ?
C4B Fe1 C1A 155.44(15) . . ?
C4A Fe1 C1A 68.54(13) . . ?
C2A Fe1 C1A 40.45(13) . . ?
C5A Fe1 C1A 40.85(13) . . ?
C5B Fe1 C1A 163.77(14) . . ?
C1B Fe1 C1A 127.44(13) . . ?
C3B Fe1 Fe1 76.08(12) . 5_655 ?
C2B Fe1 Fe1 78.70(10) . 5_655 ?
C3A Fe1 Fe1 87.93(11) . 5_655 ?
C4B Fe1 Fe1 112.29(13) . 5_655 ?
C4A Fe1 Fe1 109.59(10) . 5_655 ?
C2A Fe1 Fe1 47.21(10) . 5_655 ?
C5A Fe1 Fe1 85.78(9) . 5_655 ?
C5B Fe1 Fe1 142.50(10) . 5_655 ?
C1B Fe1 Fe1 116.46(10) . 5_655 ?
C1A Fe1 Fe1 45.39(9) . 5_655 ?
C2A C1A C5A 107.4(3) . . ?
C2A C1A C7 128.1(3) . . ?
C5A C1A C7 124.5(3) . . ?
C2A C1A Fe1 69.43(17) . . ?
C5A C1A Fe1 69.24(17) . . ?
C7 C1A Fe1 128.6(2) . . ?
C1A C2A C3A 107.7(3) . . ?
C1A C2A Fe1 70.12(17) . . ?
C3A C2A Fe1 69.02(19) . . ?
C4A C3A C2A 108.7(3) . . ?
C4A C3A Fe1 70.1(2) . . ?
C2A C3A Fe1 70.10(18) . . ?
C3A C4A C5A 107.8(3) . . ?
C3A C4A Fe1 69.45(19) . . ?
C5A C4A Fe1 70.01(18) . . ?
C4A C5A C1A 108.4(3) . . ?
C4A C5A Fe1 69.57(19) . . ?
C1A C5A Fe1 69.91(17) . . ?
C5B C1B C2B 107.6(3) . . ?
C5B C1B Fe1 69.75(19) . . ?
C2B C1B Fe1 68.99(19) . . ?
C3B C2B C1B 108.1(3) . . ?
C3B C2B Fe1 69.7(2) . . ?
C1B C2B Fe1 70.64(19) . . ?
C2B C3B C4B 107.8(3) . . ?
C2B C3B Fe1 70.0(2) . . ?
C4B C3B Fe1 70.2(2) . . ?
C5B C4B C3B 107.9(3) . . ?
C5B C4B Fe1 70.32(19) . . ?
C3B C4B Fe1 69.2(2) . . ?
C4B C5B C1B 108.6(3) . . ?
C4B C5B Fe1 69.82(19) . . ?
C1B C5B Fe1 70.24(18) . . ?
C2 N1 C1 110.9(2) . . ?
C4 N2 C5 113.5(2) . . ?
C7 N3 C3 116.1(2) . . ?
N1 C1 C5 111.1(2) . 5_655 ?
N1 C2 C3 112.2(2) . . ?
N3 C3 C4 107.8(2) . . ?
N3 C3 C6 115.3(3) . . ?
C4 C3 C6 105.5(3) . . ?
N3 C3 C2 108.8(2) . . ?
C4 C3 C2 110.9(2) . . ?
C6 C3 C2 108.5(3) . . ?
N2 C4 C3 113.8(2) . . ?
N2 C5 C1 110.6(3) . 5_655 ?
N3 C7 C1A 111.7(3) . . ?
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
Fe1 C3B 2.025(4) . ?
Fe1 C2B 2.030(3) . ?
Fe1 C3A 2.030(3) . ?
Fe1 C4B 2.038(3) . ?
Fe1 C4A 2.039(3) . ?
Fe1 C2A 2.045(3) . ?
Fe1 C5A 2.045(3) . ?
Fe1 C5B 2.045(3) . ?
Fe1 C1B 2.051(3) . ?
Fe1 C1A 2.054(3) . ?
Fe1 Fe1 14.518(4) 5_655 ?
C1A C2A 1.417(5) . ?
C1A C5A 1.430(4) . ?
C1A C7 1.494(4) . ?
C2A C3A 1.423(5) . ?
C3A C4A 1.407(5) . ?
C4A C5A 1.411(5) . ?
C1B C5B 1.402(5) . ?
C1B C2B 1.409(5) . ?
C2B C3B 1.398(6) . ?
C3B C4B 1.412(6) . ?
C4B C5B 1.392(5) . ?
N1 C2 1.460(4) . ?
N1 C1 1.461(4) . ?
N2 C4 1.478(4) . ?
N2 C5 1.486(4) . ?
N3 C7 1.462(4) . ?
N3 C3 1.464(4) . ?
C1 C5 1.502(5) 5_655 ?
C2 C3 1.534(4) . ?
C3 C4 1.528(4) . ?
C3 C6 1.534(4) . ?
C5 C1 1.502(5) 5_655 ?
