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#$Date: 2016-03-21 17:52:41 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178795 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/49/4104954.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_4104954
loop_
_publ_author_name
'Suzanne M. Neville'
'Gregory J. Halder'
'Karena W. Chapman'
'Martin B. Duriska'
'Boujemaa Moubaraki'
'Keith S. Murray'
'Cameron J. Kepert'
_publ_contact_author_address
; 
School of Chemistry
University of Sydney
NSW 2006
Australia
;
_publ_contact_author_email       c.kepert@chem.usyd.edu.au
_publ_contact_author_fax         +61-2-9351-3329
_publ_contact_author_name        'Prof. Cameron J. Kepert'
_publ_contact_author_phone       +61-2-9351-5741
_publ_section_title
;
 Guest Tunable Structure and Spin Crossover Properties in a Nanoporous
 Coordination Framework Material
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12106
_journal_page_last               12108
_journal_paper_doi               10.1021/ja905360g
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C30 H32 Fe N6 O4 S2, C3 O'
_chemical_formula_sum            'C33 H32 Fe N6 O5 S2'
_chemical_formula_weight         712.62
_chemical_name_common            SCOF-2(Pr)as
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7260(10)
_cell_length_b                   14.7260(10)
_cell_length_c                   17.899(3)
_cell_measurement_reflns_used    111
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      25.82
_cell_measurement_theta_min      2.6625
_cell_volume                     3881.5(7)
_computing_cell_refinement       'SMART (BrukerAXS, 1997)'
_computing_data_collection       'SMART (BrukerAXS, 1997)'
_computing_data_reduction        'SAINT+ (BrukerAXS, 1997)'
_computing_molecular_graphics    'XPMA/ZORTEP, WebLab Viewer 3.7'
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            2335
_diffrn_reflns_theta_full        28.09
_diffrn_reflns_theta_max         28.09
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.8998
_exptl_absorpt_correction_T_min  0.8770
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       rod
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0806
_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)+(0.1501P)²+12.9789P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2323
_refine_ls_wR_factor_ref         0.3396
_reflns_number_gt                1227
_reflns_number_total             2335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905360g_si_001_5.cif
_cod_data_source_block           SCOF-2(Pr)as
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4104954
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'y, x, 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
Fe1 Fe 0.7500 0.2500 0.7500 0.0372(5) Uani 1 4 d S
S1 S 0.98433(18) 0.01567(18) 0.7500 0.165(3) Uani 1 2 d S
C1 C 0.9026(6) 0.0974(6) 0.7500 0.061(2) Uani 1 2 d S
N1 N 0.8533(4) 0.1467(4) 0.7500 0.0520(17) Uani 1 2 d S
N10 N 0.6723(3) 0.1790(3) 0.6616(2) 0.0430(11) Uani 1 1 d .
C10 C 0.5807(4) 0.1821(5) 0.6597(4) 0.0609(17) Uani 1 1 d .
H10 H 0.5502 0.2131 0.6990 0.073 Uiso 1 1 calc R
C11 C 0.5284(5) 0.1427(5) 0.6039(4) 0.0623(17) Uani 1 1 d .
H11 H 0.4641 0.1481 0.6045 0.075 Uiso 1 1 calc R
C12 C 0.5722(4) 0.0947(4) 0.5467(3) 0.0542(16) Uani 1 1 d .
C13 C 0.6658(5) 0.0962(5) 0.5470(3) 0.0616(17) Uani 1 1 d .
H13 H 0.6985 0.0689 0.5071 0.074 Uiso 1 1 calc R
C14 C 0.7122(5) 0.1372(5) 0.6048(3) 0.0606(17) Uani 1 1 d .
H14 H 0.7767 0.1353 0.6039 0.073 Uiso 1 1 calc R
C15 C 0.5183(5) 0.0475(5) 0.4845(3) 0.0614(18) Uani 1 1 d .
C16 C 0.4431(6) 0.1058(5) 0.4567(5) 0.085(3) Uani 1 1 d .
H16A H 0.4087 0.0729 0.4183 0.128 Uiso 1 1 calc R
H16B H 0.4682 0.1615 0.4351 0.128 Uiso 1 1 calc R
H16C H 0.4026 0.1213 0.4982 0.128 Uiso 1 1 calc R
O16 O 0.5822(4) 0.0296(4) 0.4262(2) 0.0849(18) Uani 1 1 d .
H16 H 0.5553 0.0296 0.3848 0.127 Uiso 1 1 calc R
C51 C 0.2500 0.2500 0.7275 0.220 Uiso 1 4 d S
C52 C 0.2904 0.1544 0.6656 0.199 Uiso 0.25 1 d P
C50 C 0.1574 0.2544 0.7820 0.226 Uiso 0.25 1 d P
O50 O 0.1370 0.3489 0.7782 0.286 Uiso 0.25 1 d P
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'
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
N1 Fe1 N1 180.000(1) 3_655 .
N1 Fe1 N10 88.20(12) 3_655 .
N1 Fe1 N10 91.80(12) . .
N1 Fe1 N10 88.20(12) 3_655 8_666
N1 Fe1 N10 91.80(12) . 8_666
N10 Fe1 N10 176.4(2) . 8_666
N1 Fe1 N10 91.80(12) 3_655 3_655
N1 Fe1 N10 88.20(12) . 3_655
N10 Fe1 N10 88.8(2) . 3_655
N10 Fe1 N10 91.3(2) 8_666 3_655
N1 Fe1 N10 91.80(12) 3_655 7_546
N1 Fe1 N10 88.20(12) . 7_546
N10 Fe1 N10 91.3(2) . 7_546
N10 Fe1 N10 88.8(2) 8_666 7_546
N10 Fe1 N10 176.4(2) 3_655 7_546
N1 C1 S1 180.0(11) . .
C1 N1 Fe1 180.0(7) . .
C14 N10 C10 116.1(5) . .
C14 N10 Fe1 122.5(4) . .
C10 N10 Fe1 121.1(4) . .
N10 C10 C11 123.9(6) . .
N10 C10 H10 118.1 . .
C11 C10 H10 118.1 . .
C10 C11 C12 118.8(6) . .
C10 C11 H11 120.6 . .
C12 C11 H11 120.6 . .
C13 C12 C11 116.7(5) . .
C13 C12 C15 121.8(6) . .
C11 C12 C15 121.4(6) . .
C12 C13 C14 120.3(6) . .
C12 C13 H13 119.8 . .
C14 C13 H13 119.8 . .
N10 C14 C13 123.9(6) . .
N10 C14 H14 118.0 . .
C13 C14 H14 118.0 . .
O16 C15 C16 110.6(6) . .
O16 C15 C12 105.8(5) . .
C16 C15 C12 111.5(6) . .
O16 C15 C15 108.3(8) . 9_656
C16 C15 C15 111.7(8) . 9_656
C12 C15 C15 108.6(6) . 9_656
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 O16 H16 109.5 . .
C50 C51 C52 75.385(8) 3 2
C50 C51 C52 93.230(6) 4 2
C50 C51 C52 159.244(1) . 2
C50 C51 C52 128.787(3) 2 2
C50 C51 C52 159.245(1) 3 4
C50 C51 C52 128.785(3) 4 4
C50 C51 C52 75.385(8) . 4
C50 C51 C52 93.229(6) 2 4
C50 C51 C52 128.786(3) 3 3
C50 C51 C52 75.384(8) 4 3
C50 C51 C52 93.230(6) . 3
C50 C51 C52 159.243(1) 2 3
C50 C51 C52 93.231(6) 3 .
C50 C51 C52 159.244(1) 4 .
C50 C51 C52 128.787(3) . .
C50 C51 C52 75.384(8) 2 .
O50 C50 C51 100.444(1) . .
C51 C50 O50 89.0 . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 2.151(9) 3_655
Fe1 N1 2.151(9) .
Fe1 N10 2.215(4) .
Fe1 N10 2.215(4) 8_666
Fe1 N10 2.215(4) 3_655
Fe1 N10 2.215(4) 7_546
S1 C1 1.702(12) .
C1 N1 1.028(13) .
N10 C14 1.325(7) .
N10 C10 1.351(8) .
C10 C11 1.388(8) .
C10 H10 0.9500 .
C11 C12 1.402(9) .
C11 H11 0.9500 .
C12 C13 1.378(9) .
C12 C15 1.534(8) .
C13 C14 1.381(8) .
C13 H13 0.9500 .
C14 H14 0.9500 .
C15 O16 1.429(8) .
C15 C16 1.488(11) .
C15 C15 1.598(13) 9_656
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
O16 H16 0.8400 .
C51 C50 1.67735(11) 3
C51 C52 1.88721(12) 2
C50 O50 1.4254 .
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
O16 H16 S1 0.84 2.49 3.309(5) 164.7 10_666
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C10 N10 N10 C10 -65.6(9) 8_666 8_666
