#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:16:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179405 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/02/4330243.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_4330243
loop_
_publ_author_name
'Jian-Bin Lin'
'Wei Xue'
'Bao-Ying Wang'
'Jun Tao'
'Wei-Xiong Zhang'
'Jie-Peng Zhang'
'Xiao-Ming Chen'
_publ_section_title
;
 Chemical/Physical Pressure Tunable Spin-Transition Temperature and
 Hysteresis in a Two-Step Spin Crossover Porous Coordination Framework
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9423
_journal_page_last               9430
_journal_paper_doi               10.1021/ic301237p
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C24 H14 Br2 Fe N10'
_chemical_formula_weight         658.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.885(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4361(11)
_cell_length_b                   14.4264(18)
_cell_length_c                   10.2503(13)
_cell_measurement_reflns_used    995
_cell_measurement_temperature    97(2)
_cell_measurement_theta_max      22.6335
_cell_measurement_theta_min      2.4795
_cell_volume                     1216.1(3)
_computing_cell_refinement       'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.'
_computing_data_collection       'SMART Bruker AXS Inc., 1998.'
_computing_data_reduction        'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.'
_computing_molecular_graphics    'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_diffrn_ambient_temperature      97(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex CCd'
_diffrn_measurement_method       'ω scan'
_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  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7270
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    3.942
_exptl_absorpt_correction_T_max  0.8273
_exptl_absorpt_correction_T_min  0.7433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.891
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0830P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1419
_reflns_number_gt                1805
_reflns_number_total             2392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301237p_si_002_9.cif
_cod_data_source_block           1_97K
_cod_database_code               4330243
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Fe1 Fe 0.0000 1.0000 1.0000 0.0111(3) Uani 1 2 d S
Br1 Br 0.36487(7) 1.17566(4) 1.48730(5) 0.0212(2) Uani 1 1 d .
N1 N 0.2007(5) 1.0258(3) 1.1428(4) 0.0142(10) Uani 1 1 d .
N2 N 0.1545(5) 0.9194(3) 0.9348(4) 0.0114(9) Uani 1 1 d .
N3 N 0.1539(5) 0.8595(3) 0.8336(4) 0.0123(9) Uani 1 1 d .
N4 N 0.4082(5) 0.8592(3) 0.9697(4) 0.0123(9) Uani 1 1 d .
N5 N 0.4440(5) 0.6076(3) 0.6162(4) 0.0135(10) Uani 1 1 d .
C1 C 0.2132(6) 1.0830(3) 1.2483(5) 0.0141(12) Uani 1 1 d .
H1A H 0.1209 1.1178 1.2579 0.017 Uiso 1 1 calc R
C2 C 0.3569(7) 1.0921(4) 1.3427(5) 0.0158(12) Uani 1 1 d .
C3 C 0.4935(7) 1.0424(4) 1.3320(6) 0.0174(12) Uani 1 1 d .
H3A H 0.5924 1.0485 1.3973 0.021 Uiso 1 1 calc R
C4 C 0.4829(7) 0.9835(4) 1.2238(5) 0.0142(12) Uani 1 1 d .
H4A H 0.5743 0.9482 1.2133 0.017 Uiso 1 1 calc R
C5 C 0.3353(6) 0.9769(4) 1.1305(5) 0.0121(11) Uani 1 1 d .
C6 C 0.3056(6) 0.9179(4) 1.0140(5) 0.0131(11) Uani 1 1 d .
C7 C 0.3079(6) 0.8246(4) 0.8591(5) 0.0133(11) Uani 1 1 d .
C8 C 0.3554(6) 0.7530(4) 0.7745(5) 0.0133(11) Uani 1 1 d .
C9 C 0.2460(6) 0.7153(4) 0.6658(5) 0.0142(11) Uani 1 1 d .
H9A H 0.1379 0.7384 0.6422 0.017 Uiso 1 1 calc R
C10 C 0.2933(6) 0.6444(4) 0.5915(5) 0.0148(11) Uani 1 1 d .
H10A H 0.2145 0.6202 0.5184 0.018 Uiso 1 1 calc R
C11 C 0.5510(6) 0.6453(4) 0.7216(5) 0.0156(12) Uani 1 1 d .
H11A H 0.6593 0.6225 0.7414 0.019 Uiso 1 1 calc R
C12 C 0.5124(7) 0.7144(4) 0.8014(6) 0.0189(13) Uani 1 1 d .
H12A H 0.5924 0.7363 0.8754 0.023 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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
N2 Fe1 N2 180.000(1) 3_577 .
N2 Fe1 N1 99.03(17) 3_577 .
N2 Fe1 N1 80.97(17) . .
N2 Fe1 N1 80.97(17) 3_577 3_577
N2 Fe1 N1 99.03(17) . 3_577
N1 Fe1 N1 180.000(1) . 3_577
N2 Fe1 N5 90.34(17) 3_577 2_556
N2 Fe1 N5 89.66(17) . 2_556
N1 Fe1 N5 90.98(17) . 2_556
N1 Fe1 N5 89.02(17) 3_577 2_556
N2 Fe1 N5 89.66(17) 3_577 4_576
N2 Fe1 N5 90.34(17) . 4_576
N1 Fe1 N5 89.02(17) . 4_576
N1 Fe1 N5 90.98(17) 3_577 4_576
N5 Fe1 N5 180.00(16) 2_556 4_576
C1 N1 C5 118.2(5) . .
C1 N1 Fe1 126.9(4) . .
C5 N1 Fe1 114.8(3) . .
N3 N2 C6 107.0(4) . .
N3 N2 Fe1 138.5(3) . .
C6 N2 Fe1 114.4(3) . .
N2 N3 C7 104.4(4) . .
C7 N4 C6 100.7(4) . .
C10 N5 C11 115.0(5) . .
C10 N5 Fe1 120.9(4) . 2_546
C11 N5 Fe1 124.1(4) . 2_546
N1 C1 C2 121.5(5) . .
N1 C1 H1A 119.3 . .
C2 C1 H1A 119.3 . .
C1 C2 C3 120.8(5) . .
C1 C2 Br1 118.7(4) . .
C3 C2 Br1 120.4(4) . .
C4 C3 C2 118.4(5) . .
C4 C3 H3A 120.8 . .
C2 C3 H3A 120.8 . .
C3 C4 C5 118.7(5) . .
C3 C4 H4A 120.6 . .
C5 C4 H4A 120.6 . .
N1 C5 C4 122.3(5) . .
N1 C5 C6 112.8(5) . .
C4 C5 C6 124.9(5) . .
N2 C6 N4 113.3(4) . .
N2 C6 C5 117.1(5) . .
N4 C6 C5 129.7(5) . .
N4 C7 N3 114.6(5) . .
N4 C7 C8 123.8(5) . .
N3 C7 C8 121.5(5) . .
C9 C8 C12 115.5(5) . .
C9 C8 C7 122.1(5) . .
C12 C8 C7 122.3(5) . .
C10 C9 C8 120.5(5) . .
C10 C9 H9A 119.7 . .
C8 C9 H9A 119.7 . .
N5 C10 C9 124.2(5) . .
N5 C10 H10A 117.9 . .
C9 C10 H10A 117.9 . .
N5 C11 C12 124.1(5) . .
N5 C11 H11A 117.9 . .
C12 C11 H11A 117.9 . .
C11 C12 C8 120.6(5) . .
C11 C12 H12A 119.7 . .
C8 C12 H12A 119.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 1.971(4) 3_577
Fe1 N2 1.971(4) .
Fe1 N1 2.011(4) .
Fe1 N1 2.011(4) 3_577
Fe1 N5 2.074(4) 2_556
Fe1 N5 2.074(4) 4_576
Br1 C2 1.900(5) .
N1 C1 1.345(6) .
N1 C5 1.366(7) .
N2 N3 1.349(6) .
N2 C6 1.350(6) .
N3 C7 1.363(6) .
N4 C7 1.350(7) .
N4 C6 1.359(7) .
N5 C10 1.348(7) .
N5 C11 1.358(7) .
N5 Fe1 2.074(4) 2_546
C1 C2 1.379(7) .
C1 H1A 0.9500 .
C2 C3 1.383(8) .
C3 C4 1.384(7) .
C3 H3A 0.9500 .
C4 C5 1.394(7) .
C4 H4A 0.9500 .
C5 C6 1.442(7) .
C7 C8 1.461(7) .
C8 C9 1.389(7) .
C8 C12 1.406(7) .
C9 C10 1.387(8) .
C9 H9A 0.9500 .
C10 H10A 0.9500 .
C11 C12 1.374(8) .
C11 H11A 0.9500 .
C12 H12A 0.9500 .
