#------------------------------------------------------------------------------
#$Date: 2018-09-10 13:15:54 +0300 (Mon, 10 Sep 2018) $
#$Revision: 210741 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/70/7117093.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_7117093
loop_
_publ_author_name
'Scottwell, Synøve Ø.'
'Elliott, Anastasia B. S.'
'Shaffer, Karl J.'
'Nafady, Ayman'
'McAdam, C. John'
'Gordon, Keith C.'
'Crowley, James D.'
_publ_section_title
;
 Chemically and electrochemically induced expansion and contraction of a
 ferrocene rotor
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   38
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              8161
_journal_page_last               8164
_journal_paper_doi               10.1039/c5cc01973g
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C22 H15 Fe I N2'
_chemical_formula_weight         490.11
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-01-29 deposited with the CCDC.
2015-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.300(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.82160(10)
_cell_length_b                   15.6040(4)
_cell_length_c                   19.8079(4)
_cell_measurement_reflns_used    13457
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.1580
_cell_measurement_theta_min      3.6040
_cell_volume                     1798.89(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.1725
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22565
_diffrn_reflns_theta_full        77.40
_diffrn_reflns_theta_max         77.40
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    20.242
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.4125
_exptl_crystal_size_mid          0.2212
_exptl_crystal_size_min          0.1068
_refine_diff_density_max         2.333
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0513
_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)+(0.1186P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1451
_reflns_number_gt                3526
_reflns_number_total             3773
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc01973g2.cif
_cod_data_source_block
c:\users\sscott\desktop\sos198\struct\tmp\sos198
_cod_database_code               7117093
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'
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
I1 I 0.46565(4) 0.419786(14) 0.229519(12) 0.01951(16) Uani 1 1 d . . .
Fe1 Fe 0.36214(9) 0.63372(3) 0.14770(3) 0.01077(17) Uani 1 1 d . . .
N1 N 0.6978(6) 0.4333(2) 0.46346(17) 0.0154(6) Uani 1 1 d . . .
N2 N 1.1460(6) 0.2824(2) 0.50734(19) 0.0212(7) Uani 1 1 d . . .
C1 C 0.1188(6) 0.5390(2) 0.1498(2) 0.0168(7) Uani 1 1 d . . .
H1 H 0.0016 0.5341 0.1822 0.020 Uiso 1 1 calc R . .
C2 C 0.1030(7) 0.5838(2) 0.0872(2) 0.0180(8) Uani 1 1 d . . .
H2 H -0.0288 0.6132 0.0700 0.022 Uiso 1 1 calc R . .
C3 C 0.3194(8) 0.5772(2) 0.0546(2) 0.0195(8) Uani 1 1 d . . .
H3 H 0.3565 0.6019 0.0124 0.023 Uiso 1 1 calc R . .
C4 C 0.4692(6) 0.5270(2) 0.0966(2) 0.0168(7) Uani 1 1 d . . .
H4 H 0.6238 0.5123 0.0874 0.020 Uiso 1 1 calc R . .
C5 C 0.3448(6) 0.5028(2) 0.15485(18) 0.0135(7) Uani 1 1 d . . .
C6 C 0.3050(6) 0.7135(2) 0.22796(19) 0.0143(7) Uani 1 1 d . . .
H6 H 0.1940 0.7053 0.2618 0.017 Uiso 1 1 calc R . .
C7 C 0.2705(6) 0.7584(2) 0.1661(2) 0.0166(7) Uani 1 1 d . . .
H7 H 0.1318 0.7854 0.1515 0.020 Uiso 1 1 calc R . .
C8 C 0.4795(6) 0.7561(2) 0.12962(19) 0.0167(7) Uani 1 1 d . . .
H8 H 0.5041 0.7814 0.0868 0.020 Uiso 1 1 calc R . .
C9 C 0.6441(6) 0.7092(2) 0.16883(19) 0.0157(7) Uani 1 1 d . . .
H9 H 0.7978 0.6974 0.1568 0.019 Uiso 1 1 calc R . .
C10 C 0.5358(6) 0.6830(2) 0.23013(18) 0.0139(6) Uani 1 1 d . . .
C11 C 0.6449(6) 0.6334(2) 0.2829(2) 0.0152(7) Uani 1 1 d . . .
C12 C 0.7334(7) 0.5895(2) 0.3254(2) 0.0158(8) Uani 1 1 d . . .
C13 C 0.6536(6) 0.4968(3) 0.4211(2) 0.0178(7) Uani 1 1 d . . .
H13 H 0.5069 0.5233 0.4228 0.021 Uiso 1 1 calc R . .
C14 C 0.8091(6) 0.5277(2) 0.37389(18) 0.0129(7) Uani 1 1 d . . .
C15 C 1.0300(6) 0.4906(3) 0.37518(19) 0.0168(7) Uani 1 1 d . . .
H15 H 1.1441 0.5105 0.3454 0.020 Uiso 1 1 calc R . .
C16 C 1.0790(7) 0.4250(2) 0.4202(2) 0.0154(7) Uani 1 1 d . . .
H16 H 1.2273 0.3996 0.4218 0.018 Uiso 1 1 calc R . .
C17 C 0.9091(6) 0.3965(2) 0.46310(18) 0.0131(6) Uani 1 1 d . . .
C18 C 0.9431(6) 0.3232(2) 0.50970(18) 0.0152(7) Uani 1 1 d . . .
C19 C 0.7679(7) 0.2983(2) 0.5532(2) 0.0192(7) Uani 1 1 d . . .
H19 H 0.6261 0.3284 0.5533 0.023 Uiso 1 1 calc R . .
C20 C 0.8050(7) 0.2291(3) 0.5962(2) 0.0218(8) Uani 1 1 d . . .
H20 H 0.6898 0.2112 0.6263 0.026 Uiso 1 1 calc R . .
C21 C 1.0149(8) 0.1866(3) 0.5940(2) 0.0282(9) Uani 1 1 d . . .
H21 H 1.0462 0.1390 0.6226 0.034 Uiso 1 1 calc R . .
C22 C 1.1773(8) 0.2154(3) 0.5490(2) 0.0261(9) Uani 1 1 d . . .
H22 H 1.3197 0.1858 0.5477 0.031 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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
C1 Fe1 C10 125.66(15) . .
C1 Fe1 C5 40.93(14) . .
C10 Fe1 C5 110.05(14) . .
C1 Fe1 C6 107.30(15) . .
C10 Fe1 C6 40.66(14) . .
C5 Fe1 C6 122.81(15) . .
C1 Fe1 C7 119.84(15) . .
C10 Fe1 C7 68.20(15) . .
C5 Fe1 C7 156.76(15) . .
C6 Fe1 C7 40.53(15) . .
C1 Fe1 C4 69.08(14) . .
C10 Fe1 C4 123.18(16) . .
C5 Fe1 C4 40.72(14) . .
C6 Fe1 C4 158.51(16) . .
C7 Fe1 C4 159.96(16) . .
C1 Fe1 C3 68.84(16) . .
C10 Fe1 C3 157.42(16) . .
C5 Fe1 C3 68.22(15) . .
C6 Fe1 C3 159.61(17) . .
C7 Fe1 C3 122.67(16) . .
C4 Fe1 C3 40.61(16) . .
C1 Fe1 C9 163.48(16) . .
C10 Fe1 C9 41.05(14) . .
C5 Fe1 C9 126.69(14) . .
C6 Fe1 C9 68.73(14) . .
C7 Fe1 C9 68.28(15) . .
C4 Fe1 C9 108.39(15) . .
C3 Fe1 C9 120.59(16) . .
C1 Fe1 C2 40.61(16) . .
C10 Fe1 C2 161.28(17) . .
C5 Fe1 C2 68.08(14) . .
C6 Fe1 C2 123.42(16) . .
C7 Fe1 C2 105.77(15) . .
C4 Fe1 C2 68.46(15) . .
C3 Fe1 C2 40.78(17) . .
C9 Fe1 C2 155.05(16) . .
C1 Fe1 C8 154.65(16) . .
C10 Fe1 C8 68.38(15) . .
C5 Fe1 C8 162.11(15) . .
C6 Fe1 C8 68.46(15) . .
C7 Fe1 C8 40.66(15) . .
C4 Fe1 C8 124.04(15) . .
C3 Fe1 C8 106.00(16) . .
C9 Fe1 C8 40.39(15) . .
C2 Fe1 C8 119.38(15) . .
C13 N1 C17 118.5(3) . .
C22 N2 C18 117.0(4) . .
C2 C1 C5 107.2(3) . .
C2 C1 Fe1 70.1(2) . .
C5 C1 Fe1 69.6(2) . .
C1 C2 C3 108.5(4) . .
C1 C2 Fe1 69.3(2) . .
C3 C2 Fe1 69.5(2) . .
C4 C3 C2 108.0(4) . .
C4 C3 Fe1 69.7(2) . .
C2 C3 Fe1 69.7(2) . .
C3 C4 C5 107.6(3) . .
C3 C4 Fe1 69.7(2) . .
C5 C4 Fe1 69.5(2) . .
C4 C5 C1 108.7(3) . .
C4 C5 Fe1 69.7(2) . .
C1 C5 Fe1 69.4(2) . .
C4 C5 I1 124.8(3) . .
C1 C5 I1 126.2(3) . .
Fe1 C5 I1 130.85(18) . .
C7 C6 C10 107.8(3) . .
C7 C6 Fe1 69.7(2) . .
C10 C6 Fe1 69.6(2) . .
C6 C7 C8 108.5(3) . .
C6 C7 Fe1 69.7(2) . .
C8 C7 Fe1 70.0(2) . .
C9 C8 C7 107.9(3) . .
C9 C8 Fe1 69.6(2) . .
C7 C8 Fe1 69.3(2) . .
C8 C9 C10 107.7(3) . .
C8 C9 Fe1 70.1(2) . .
C10 C9 Fe1 69.3(2) . .
C6 C10 C11 127.0(3) . .
C6 C10 C9 108.0(3) . .
C11 C10 C9 124.9(3) . .
C6 C10 Fe1 69.7(2) . .
C11 C10 Fe1 125.4(3) . .
C9 C10 Fe1 69.7(2) . .
C12 C11 C10 177.5(4) . .
C11 C12 C14 170.7(4) . .
N1 C13 C14 124.3(3) . .
C13 C14 C15 116.7(3) . .
C13 C14 C12 119.3(3) . .
C15 C14 C12 123.9(3) . .
C16 C15 C14 119.4(3) . .
C15 C16 C17 119.4(3) . .
N1 C17 C16 121.6(4) . .
N1 C17 C18 115.6(3) . .
C16 C17 C18 122.7(3) . .
N2 C18 C19 122.8(4) . .
N2 C18 C17 116.7(3) . .
C19 C18 C17 120.5(3) . .
C20 C19 C18 119.1(4) . .
C19 C20 C21 118.4(4) . .
C22 C21 C20 118.5(4) . .
N2 C22 C21 124.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 C5 2.077(4) .
Fe1 C1 2.048(4) .
Fe1 C10 2.050(4) .
Fe1 C5 2.051(4) .
Fe1 C6 2.052(4) .
Fe1 C7 2.053(4) .
Fe1 C4 2.053(4) .
Fe1 C3 2.054(4) .
Fe1 C9 2.056(4) .
Fe1 C2 2.058(4) .
Fe1 C8 2.063(4) .
N1 C13 1.320(5) .
N1 C17 1.357(5) .
N2 C22 1.342(6) .
N2 C18 1.343(5) .
C1 C2 1.425(6) .
C1 C5 1.433(5) .
C2 C3 1.432(6) .
C3 C4 1.425(6) .
C4 C5 1.428(5) .
C6 C7 1.422(5) .
C6 C10 1.425(5) .
C7 C8 1.430(5) .
C8 C9 1.422(5) .
C9 C10 1.440(5) .
C10 C11 1.437(5) .
C11 C12 1.192(6) .
C12 C14 1.424(5) .
C13 C14 1.402(5) .
C14 C15 1.410(5) .
C15 C16 1.383(6) .
C16 C17 1.391(5) .
C17 C18 1.481(5) .
C18 C19 1.405(5) .
C19 C20 1.389(6) .
C20 C21 1.392(7) .
C21 C22 1.389(7) .
