#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:05:57 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180222 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/08/7110815.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_7110815
loop_
_publ_author_name
'MacGillivray, Leonard R.'
'Spinney, Heather A.'
'Reid, Jennifer L.'
'Ripmeester, John A.'
_publ_section_title
;
 Entrapment of ferrocenes within supramolecular, deep-cavity
 resorcin[4]arenes
;
_journal_issue                   6
_journal_name_full               'Chemical Communications'
_journal_page_first              517
_journal_paper_doi               10.1039/a909745g
_journal_year                    2000
_chemical_formula_sum            'C62 H58 Fe N4 O8'
_chemical_formula_weight         1043.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.710(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7302(13)
_cell_length_b                   25.440(3)
_cell_length_c                   10.8246(14)
_cell_measurement_temperature    173(2)
_cell_volume                     2506.3(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1766
_diffrn_reflns_av_sigmaI/netI    0.1726
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11030
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.354
_exptl_crystal_density_diffrn    1.38
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         3370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1986
_refine_ls_R_factor_gt           0.0900
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1261P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2075
_refine_ls_wR_factor_ref         0.2451
_reflns_number_gt                1527
_reflns_number_total             3370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909745gsup1.cif
_cod_data_source_block           test
_cod_original_cell_volume        2506.4(6)
_cod_original_sg_symbol_H-M      P21/m
_cod_database_code               7110815
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
Fe Fe 0.3076(2) 0.7500 0.1850(2) 0.0644(8) Uani 1 2 d S
O1 O 0.4713(6) 0.9183(2) 0.5938(5) 0.0437(15) Uani 1 1 d .
H1 H 0.3980 0.9294 0.5313 0.052 Uiso 1 1 calc R
O2 O 0.6926(6) 0.9244(2) 0.2601(5) 0.0439(16) Uani 1 1 d .
H2 H 0.6115 0.9384 0.2173 0.053 Uiso 1 1 calc R
O3 O 0.3872(6) 0.8425(2) 0.7449(6) 0.0487(16) Uani 1 1 d .
H3 H 0.4186 0.8671 0.7102 0.058 Uiso 1 1 calc R
O4 O 0.7326(7) 0.8422(2) 0.1113(5) 0.0480(16) Uani 1 1 d .
H4 H 0.7274 0.8670 0.1605 0.058 Uiso 1 1 calc R
N1 N 0.2324(7) 0.9582(3) 0.3961(7) 0.0447(19) Uani 1 1 d .
N2 N -0.4368(8) 1.0363(3) -0.0985(7) 0.0437(19) Uani 1 1 d .
C1 C 0.5798(8) 0.9031(3) 0.5457(8) 0.033(2) Uani 1 1 d .
C2 C 0.5811(9) 0.9220(3) 0.4260(8) 0.037(2) Uani 1 1 d .
H2 H 0.5075 0.9460 0.3765 0.044 Uiso 1 1 calc R
C3 C 0.6892(8) 0.9059(3) 0.3776(7) 0.031(2) Uani 1 1 d .
C4 C 0.7973(8) 0.8701(3) 0.4495(7) 0.028(2) Uani 1 1 d .
C5 C 0.7941(9) 0.8536(3) 0.5682(8) 0.034(2) Uani 1 1 d .
H5 H 0.8689 0.8301 0.6186 0.040 Uiso 1 1 calc R
C6 C 0.6872(8) 0.8691(3) 0.6213(7) 0.0252(19) Uani 1 1 d .
C7 C 0.6941(8) 0.8496(3) 0.7579(7) 0.032(2) Uani 1 1 d .
H7 H 0.6427 0.8766 0.7928 0.038 Uiso 1 1 calc R
C8 C 0.8520(8) 0.8464(3) 0.8568(7) 0.037(2) Uani 1 1 d .
H8C H 0.9013 0.8802 0.8597 0.044 Uiso 1 1 calc R
H8B H 0.9053 0.8188 0.8292 0.044 Uiso 1 1 calc R
H8A H 0.8504 0.8381 0.9447 0.044 Uiso 1 1 calc R
C9 C 0.6093(8) 0.7982(3) 0.7480(7) 0.0278(19) Uani 1 1 d .
C10 C 0.4656(9) 0.7972(3) 0.7451(8) 0.040(2) Uani 1 1 d .
C11 C 0.3957(13) 0.7500 0.7451(12) 0.048(4) Uani 1 2 d S
H11 H 0.2981 0.7500 0.7452 0.058 Uiso 1 2 calc SR
C12 C 0.6781(12) 0.7500 0.7500(10) 0.031(3) Uani 1 2 d S
H12 H 0.7768 0.7500 0.7530 0.037 Uiso 1 2 calc SR
C13 C 0.9135(8) 0.8502(3) 0.3954(8) 0.033(2) Uani 1 1 d .
H13 H 0.9185 0.8768 0.3290 0.040 Uiso 1 1 calc R
C14 C 1.0669(8) 0.8479(3) 0.5012(8) 0.043(2) Uani 1 1 d .
H14C H 1.0656 0.8245 0.5727 0.051 Uiso 1 1 calc R
H14B H 1.0967 0.8832 0.5367 0.051 Uiso 1 1 calc R
H14A H 1.1368 0.8345 0.4622 0.051 Uiso 1 1 calc R
C15 C 0.8650(8) 0.7987(3) 0.3202(8) 0.0297(19) Uani 1 1 d .
C16 C 0.7826(9) 0.7969(4) 0.1875(9) 0.040(2) Uani 1 1 d .
C17 C 0.7389(13) 0.7500 0.1202(12) 0.042(3) Uani 1 2 d S
H17 H 0.6797 0.7500 0.0291 0.051 Uiso 1 2 calc SR
C18 C 0.9047(12) 0.7500 0.3832(11) 0.032(3) Uani 1 2 d S
H18 H 0.9623 0.7500 0.4747 0.039 Uiso 1 2 calc SR
C19 C 0.1850(10) 0.9381(4) 0.2744(9) 0.051(3) Uani 1 1 d .
H19 H 0.2450 0.9125 0.2541 0.061 Uiso 1 1 calc R
C20 C 0.0559(9) 0.9516(4) 0.1768(8) 0.048(2) Uani 1 1 d .
H20 H 0.0295 0.9352 0.0928 0.057 Uiso 1 1 calc R
C21 C -0.0360(9) 0.9886(3) 0.1984(8) 0.035(2) Uani 1 1 d .
C22 C 0.0138(10) 1.0100(3) 0.3244(10) 0.051(3) Uani 1 1 d .
H22 H -0.0418 1.0366 0.3469 0.061 Uiso 1 1 calc R
C23 C 0.1456(11) 0.9926(4) 0.4182(9) 0.053(3) Uani 1 1 d .
H23 H 0.1735 1.0069 0.5047 0.064 Uiso 1 1 calc R
C24 C -0.1730(9) 1.0045(3) 0.0971(8) 0.033(2) Uani 1 1 d .
C25 C -0.2479(9) 0.9734(3) -0.0083(9) 0.040(2) Uani 1 1 d .
H25 H -0.2108 0.9395 -0.0164 0.048 Uiso 1 1 calc R
C26 C -0.3766(10) 0.9906(3) -0.1028(9) 0.045(2) Uani 1 1 d .
H26 H -0.4244 0.9680 -0.1752 0.054 Uiso 1 1 calc R
C27 C -0.2407(10) 1.0540(3) 0.1008(9) 0.048(2) Uani 1 1 d .
H27 H -0.1961 1.0775 0.1718 0.058 Uiso 1 1 calc R
C28 C -0.3661(10) 1.0673(4) 0.0054(9) 0.050(2) Uani 1 1 d .
H28 H -0.4078 1.1006 0.0110 0.059 Uiso 1 1 calc R
C29 C 0.2307(16) 0.8128(6) 0.073(2) 0.135(8) Uani 1 1 d .
H29 H 0.1677 0.8141 -0.0171 0.162 Uiso 1 1 calc R
C30 C 0.1814(15) 0.8127(6) 0.174(2) 0.153(9) Uani 1 1 d .
H30 H 0.0819 0.8140 0.1689 0.183 Uiso 1 1 calc R
C31 C 0.320(2) 0.8101(7) 0.3016(19) 0.182(9) Uani 1 1 d .
H31 H 0.3242 0.8089 0.3907 0.219 Uiso 1 1 calc R
C32 C 0.433(2) 0.8100(7) 0.255(3) 0.201(14) Uani 1 1 d .
H32 H 0.5330 0.8094 0.3120 0.241 Uiso 1 1 calc R
C33 C 0.390(3) 0.8108(8) 0.115(3) 0.211(15) Uani 1 1 d .
H33 H 0.4504 0.8101 0.0619 0.253 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'
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
C32 Fe C32 104.2(15) . 4_575
C32 Fe C31 41.1(8) . .
C32 Fe C31 118.5(10) 4_575 .
C32 Fe C31 118.5(10) . 4_575
C32 Fe C31 41.1(8) 4_575 4_575
C31 Fe C31 102.6(14) . 4_575
C32 Fe C29 157.5(8) . 4_575
C32 Fe C29 69.7(11) 4_575 4_575
C31 Fe C29 160.9(7) . 4_575
C31 Fe C29 71.9(9) 4_575 4_575
C32 Fe C29 69.7(11) . .
C32 Fe C29 157.5(8) 4_575 .
C31 Fe C29 71.9(9) . .
C31 Fe C29 160.9(7) 4_575 .
C29 Fe C29 107.2(13) 4_575 .
C32 Fe C30 161.1(11) . 4_575
C32 Fe C30 71.4(8) 4_575 4_575
C31 Fe C30 123.9(9) . 4_575
C31 Fe C30 46.2(7) 4_575 4_575
C29 Fe C30 39.5(7) 4_575 4_575
C29 Fe C30 121.2(6) . 4_575
C32 Fe C30 71.4(8) . .
C32 Fe C30 161.1(11) 4_575 .
C31 Fe C30 46.2(7) . .
C31 Fe C30 123.9(9) 4_575 .
C29 Fe C30 121.2(6) 4_575 .
C29 Fe C30 39.5(7) . .
C30 Fe C30 106.5(10) 4_575 .
C32 Fe C33 42.4(9) . .
C32 Fe C33 118.2(6) 4_575 .
C31 Fe C33 72.8(11) . .
C31 Fe C33 154.5(9) 4_575 .
C29 Fe C33 120.1(10) 4_575 .
C29 Fe C33 42.7(7) . .
C30 Fe C33 156.0(11) 4_575 .
C30 Fe C33 71.5(9) . .
C32 Fe C33 118.2(6) . 4_575
C32 Fe C33 42.4(9) 4_575 4_575
C31 Fe C33 154.5(9) . 4_575
C31 Fe C33 72.8(11) 4_575 4_575
C29 Fe C33 42.7(7) 4_575 4_575
C29 Fe C33 120.1(10) . 4_575
C30 Fe C33 71.5(9) 4_575 4_575
C30 Fe C33 156.0(11) . 4_575
C33 Fe C33 100.3(15) . 4_575
C23 N1 C19 114.9(8) . .
C26 N2 C28 116.6(7) . .
C6 C1 C2 121.1(8) . .
C6 C1 O1 117.9(7) . .
C2 C1 O1 121.0(7) . .
C1 C2 C3 120.6(8) . .
O2 C3 C2 121.3(7) . .
O2 C3 C4 118.7(7) . .
C2 C3 C4 120.0(7) . .
C5 C4 C3 117.5(7) . .
C5 C4 C13 121.7(7) . .
C3 C4 C13 120.9(7) . .
C4 C5 C6 124.4(8) . .
C1 C6 C5 116.5(7) . .
C1 C6 C7 122.6(7) . .
C5 C6 C7 120.9(7) . .
C8 C7 C9 112.7(6) . .
C8 C7 C6 112.4(6) . .
C9 C7 C6 111.7(6) . .
C10 C9 C12 117.3(8) . .
C10 C9 C7 122.1(7) . .
C12 C9 C7 120.4(8) . .
C11 C10 O3 117.0(8) . .
C11 C10 C9 120.6(9) . .
O3 C10 C9 122.4(8) . .
C10 C11 C10 120.9(12) . 4_575
C9 C12 C9 123.3(11) . 4_575
C15 C13 C14 113.7(7) . .
C15 C13 C4 110.9(6) . .
C14 C13 C4 112.6(7) . .
C16 C15 C18 115.9(8) . .
C16 C15 C13 122.7(7) . .
C18 C15 C13 121.4(7) . .
C15 C16 C17 122.3(9) . .
C15 C16 O4 122.7(8) . .
C17 C16 O4 114.9(8) . .
C16 C17 C16 119.1(12) . 4_575
C15 C18 C15 124.3(11) 4_575 .
N1 C19 C20 124.6(8) . .
C19 C20 C21 121.0(8) . .
C20 C21 C22 114.5(8) . .
C20 C21 C24 122.8(8) . .
C22 C21 C24 122.8(8) . .
C21 C22 C23 120.1(8) . .
N1 C23 C22 124.8(9) . .
C25 C24 C27 114.7(7) . .
C25 C24 C21 123.0(8) . .
C27 C24 C21 122.3(8) . .
C24 C25 C26 120.8(8) . .
N2 C26 C25 123.7(8) . .
C28 C27 C24 120.5(8) . .
C27 C28 N2 123.6(8) . .
C30 C29 C33 113(2) . .
C30 C29 Fe 70.4(10) . .
C33 C29 Fe 69.6(8) . .
C29 C30 C31 106.2(15) . .
C29 C30 Fe 70.1(8) . .
C31 C30 Fe 65.9(7) . .
C32 C31 C30 103(2) . .
C32 C31 Fe 68.4(9) . .
C30 C31 Fe 68.0(7) . .
C31 C32 C33 115(2) . .
C31 C32 Fe 70.5(10) . .
C33 C32 Fe 71.8(12) . .
C32 C33 C29 102(2) . .
C32 C33 Fe 65.8(10) . .
C29 C33 Fe 67.7(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe C32 1.934(15) .
Fe C32 1.934(15) 4_575
Fe C31 1.960(13) .
Fe C31 1.960(13) 4_575
Fe C29 1.987(13) 4_575
Fe C29 1.987(13) .
Fe C30 1.992(13) 4_575
Fe C30 1.992(13) .
Fe C33 2.013(16) .
Fe C33 2.013(16) 4_575
O1 C1 1.387(9) .
O2 C3 1.366(8) .
O3 C10 1.382(9) .
O4 C16 1.400(9) .
N1 C23 1.295(10) .
N1 C19 1.334(11) .
N2 C26 1.310(10) .
N2 C28 1.347(10) .
C1 C6 1.381(10) .
C1 C2 1.386(10) .
C2 C3 1.392(10) .
C3 C4 1.401(10) .
C4 C5 1.363(10) .
C4 C13 1.531(10) .
C5 C6 1.411(10) .
C6 C7 1.538(10) .
C7 C8 1.533(10) .
C7 C9 1.530(10) .
C9 C10 1.388(10) .
C9 C12 1.394(9) .
C10 C11 1.380(10) .
C11 C10 1.380(10) 4_575
C12 C9 1.394(9) 4_575
C13 C15 1.527(11) .
C13 C14 1.528(10) .
C15 C16 1.377(11) .
C15 C18 1.401(9) .
C16 C17 1.384(10) .
C17 C16 1.384(10) 4_575
C18 C15 1.401(9) 4_575
C19 C20 1.369(11) .
C20 C21 1.374(11) .
C21 C22 1.388(11) .
C21 C24 1.452(11) .
C22 C23 1.397(12) .
C24 C25 1.367(11) .
C24 C27 1.427(11) .
C25 C26 1.379(11) .
C27 C28 1.334(11) .
C29 C30 1.34(2) .
C29 C33 1.46(2) .
C30 C31 1.55(2) .
C31 C32 1.37(2) .
C32 C33 1.43(3) .
