#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:54:05 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180280 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/66/7116642.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_7116642
loop_
_publ_author_name
'Dong Shao'
'Shao-Liang Zhang'
'Xin-Hua Zhao'
'Xin-Yi Wang'
_publ_section_title
;
 Spin canting, metamagnetism, and single-chain magnetic behaviour in a
 cyano-bridged homospin iron(II) compound
;
_journal_name_full               Chem.Commun.
_journal_page_first              4360
_journal_paper_doi               10.1039/C4cc10003D
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C16 H23 B F4 Fe N6'
_chemical_formula_weight         442.06
_chemical_name_systematic
; 
[Fe(LN5)(CN)][BF4] 
;
_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
_audit_update_record
;
2014-10-24 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.336(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0808(11)
_cell_length_b                   10.6982(9)
_cell_length_c                   14.0524(12)
_cell_measurement_temperature    296(2)
_cell_volume                     1954.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4439
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.8866
_exptl_absorpt_correction_T_min  0.5591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS;Bruker,2000
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4439
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0438
_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)+(0.0711P)²+1.0038P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1302
_reflns_number_gt                3659
_reflns_number_total             4439
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc10003d2.cif
_cod_data_source_block           c:\users\admini~1\desktop\last\bf4\t5
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               7116642
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 0.73498(3) 0.54167(3) 0.23051(3) 0.03091(13) Uani 1 1 d .
N6 N 0.71617(19) 0.3387(2) 0.21115(18) 0.0449(6) Uani 1 1 d .
C3 C 0.6089(2) 0.6267(2) 0.0438(2) 0.0427(7) Uani 1 1 d .
C2 C 0.5238(3) 0.6630(3) -0.0192(3) 0.0621(10) Uani 1 1 d .
H3A H 0.5307 0.6811 -0.0829 0.075 Uiso 1 1 calc R
C1 C 0.4300(3) 0.6710(3) 0.0153(3) 0.0681(11) Uani 1 1 d .
H4A H 0.3721 0.6923 -0.0260 0.082 Uiso 1 1 calc R
C15 C 0.4205(3) 0.6482(3) 0.1095(3) 0.0619(10) Uani 1 1 d .
H5A H 0.3571 0.6556 0.1330 0.074 Uiso 1 1 calc R
C14 C 0.5086(2) 0.6133(3) 0.1704(2) 0.0413(6) Uani 1 1 d .
C12 C 0.5109(2) 0.5864(3) 0.2735(3) 0.0473(7) Uani 1 1 d .
C11 C 0.6132(4) 0.5199(4) 0.4164(3) 0.0705(11) Uani 1 1 d .
H8A H 0.5923 0.4341 0.4253 0.085 Uiso 1 1 calc R
H8B H 0.5719 0.5738 0.4525 0.085 Uiso 1 1 calc R
C10 C 0.7247(4) 0.5354(4) 0.4516(3) 0.0733(12) Uani 1 1 d .
H9A H 0.7416 0.6236 0.4569 0.088 Uiso 1 1 calc R
H9B H 0.7391 0.4978 0.5144 0.088 Uiso 1 1 calc R
C9 C 0.8976(3) 0.4882(4) 0.4061(3) 0.0759(13) Uani 1 1 d .
H10A H 0.9212 0.4391 0.4623 0.091 Uiso 1 1 calc R
H10B H 0.9151 0.5750 0.4195 0.091 Uiso 1 1 calc R
C8 C 0.9490(3) 0.4443(4) 0.3229(4) 0.0807(15) Uani 1 1 d .
H11A H 1.0228 0.4561 0.3359 0.097 Uiso 1 1 calc R
H11B H 0.9359 0.3558 0.3126 0.097 Uiso 1 1 calc R
C7 C 0.9333(3) 0.4594(4) 0.1464(4) 0.0721(13) Uani 1 1 d .
H12A H 0.9059 0.3752 0.1403 0.086 Uiso 1 1 calc R
H12B H 1.0072 0.4553 0.1449 0.086 Uiso 1 1 calc R
C6 C 0.8855(3) 0.5390(4) 0.0656(3) 0.0727(12) Uani 1 1 d .
H13A H 0.9232 0.6168 0.0632 0.087 Uiso 1 1 calc R
H13B H 0.8875 0.4958 0.0052 0.087 Uiso 1 1 calc R
C4 C 0.7134(3) 0.6095(3) 0.0161(2) 0.0500(8) Uani 1 1 d .
C5 C 0.7367(4) 0.6461(5) -0.0824(3) 0.0914(15) Uani 1 1 d .
H15A H 0.8076 0.6287 -0.0888 0.137 Uiso 1 1 calc R
H15B H 0.7238 0.7338 -0.0919 0.137 Uiso 1 1 calc R
H15C H 0.6936 0.5993 -0.1293 0.137 Uiso 1 1 calc R
C13 C 0.4136(3) 0.6016(5) 0.3208(4) 0.0882(14) Uani 1 1 d .
H16A H 0.4271 0.5810 0.3875 0.132 Uiso 1 1 calc R
H16B H 0.3615 0.5469 0.2908 0.132 Uiso 1 1 calc R
H16C H 0.3904 0.6866 0.3142 0.132 Uiso 1 1 calc R
C16 C 0.77200(19) 0.7346(2) 0.27365(18) 0.0329(5) Uani 1 1 d .
N1 N 0.60025(17) 0.60187(18) 0.13613(16) 0.0338(5) Uani 1 1 d .
N5 N 0.5971(2) 0.5526(2) 0.31452(19) 0.0451(6) Uani 1 1 d .
N4 N 0.7867(2) 0.4755(2) 0.3847(2) 0.0569(8) Uani 1 1 d .
H4 H 0.7727 0.3923 0.3864 0.068 Uiso 1 1 calc R
N3 N 0.9099(2) 0.5147(3) 0.2365(3) 0.0577(8) Uani 1 1 d .
H5 H 0.9394 0.5919 0.2410 0.069 Uiso 1 1 calc R
N2 N 0.7778(2) 0.5647(2) 0.0819(2) 0.0470(6) Uani 1 1 d .
B1 B 0.1291(4) 0.7375(5) 0.1643(4) 0.0683(12) Uani 1 1 d .
F1 F 0.0603(3) 0.7549(5) 0.2261(4) 0.179(2) Uani 1 1 d .
F2 F 0.0752(4) 0.7572(6) 0.0772(3) 0.197(2) Uani 1 1 d .
F3 F 0.1594(3) 0.6223(4) 0.1665(5) 0.189(2) Uani 1 1 d .
F4 F 0.2103(2) 0.8163(3) 0.1811(3) 0.1109(10) Uani 1 1 d .
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
N1 Fe1 C16 91.67(8) .
N1 Fe1 N6 98.30(8) .
C16 Fe1 N6 169.46(9) .
N1 Fe1 N2 70.65(10) .
C16 Fe1 N2 94.82(10) .
N6 Fe1 N2 91.70(10) .
N1 Fe1 N5 70.45(9) .
C16 Fe1 N5 88.36(9) .
N6 Fe1 N5 91.77(9) .
N2 Fe1 N5 141.04(11) .
N1 Fe1 N3 142.47(11) .
C16 Fe1 N3 85.36(9) .
N6 Fe1 N3 88.75(9) .
N2 Fe1 N3 72.34(12) .
N5 Fe1 N3 146.53(11) .
N1 Fe1 N4 142.58(11) .
C16 Fe1 N4 89.78(9) .
N6 Fe1 N4 80.24(9) .
N2 Fe1 N4 146.41(12) .
N5 Fe1 N4 72.22(11) .
N3 Fe1 N4 74.91(12) .
C16 N6 Fe1 158.4(2) 2_645
N1 C3 C2 121.4(3) .
N1 C3 C4 114.3(3) .
C2 C3 C4 124.3(3) .
C1 C2 C3 118.4(3) .
C15 C1 C2 120.8(3) .
C1 C15 C14 118.7(3) .
N1 C14 C15 120.6(3) .
N1 C14 C12 114.3(3) .
C15 C14 C12 125.1(3) .
N5 C12 C14 115.2(3) .
N5 C12 C13 125.8(3) .
C14 C12 C13 119.1(3) .
N5 C11 C10 109.0(3) .
N4 C10 C11 109.3(3) .
N4 C9 C8 109.6(3) .
N3 C8 C9 109.9(3) .
N3 C7 C6 108.4(3) .
N2 C6 C7 108.2(3) .
N2 C4 C3 114.4(3) .
N2 C4 C5 125.6(4) .
C3 C4 C5 120.0(4) .
N6 C16 Fe1 173.0(2) 2_655
C3 N1 C14 120.1(2) .
C3 N1 Fe1 119.83(19) .
C14 N1 Fe1 120.04(19) .
C12 N5 C11 122.6(3) .
C12 N5 Fe1 120.0(2) .
C11 N5 Fe1 117.4(3) .
C9 N4 C10 116.1(3) .
C9 N4 Fe1 110.3(2) .
C10 N4 Fe1 110.1(2) .
C7 N3 C8 114.9(3) .
C7 N3 Fe1 108.8(2) .
C8 N3 Fe1 110.4(3) .
C4 N2 C6 121.5(3) .
C4 N2 Fe1 120.4(2) .
C6 N2 Fe1 117.8(3) .
F3 B1 F1 110.1(5) .
F3 B1 F4 110.9(4) .
F1 B1 F4 111.9(4) .
F3 B1 F2 107.3(5) .
F1 B1 F2 104.1(5) .
F4 B1 F2 112.3(5) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 2.183(2) .
Fe1 C16 2.190(2) .
Fe1 N6 2.199(2) .
Fe1 N2 2.234(3) .
Fe1 N5 2.265(3) .
Fe1 N3 2.299(3) .
Fe1 N4 2.309(3) .
N6 C16 1.142(3) 2_645
C3 N1 1.341(4) .
C3 C2 1.399(4) .
C3 C4 1.473(5) .
C2 C1 1.371(6) .
C1 C15 1.366(6) .
C15 C14 1.408(4) .
C14 N1 1.345(4) .
C14 C12 1.474(5) .
C12 N5 1.261(4) .
C12 C13 1.509(4) .
C11 N5 1.466(4) .
C11 C10 1.497(7) .
C10 N4 1.457(5) .
C9 N4 1.455(5) .
C9 C8 1.487(7) .
C8 N3 1.472(6) .
C7 N3 1.460(6) .
C7 C6 1.499(7) .
C6 N2 1.478(4) .
C4 N2 1.275(5) .
C4 C5 1.501(5) .
C16 N6 1.142(3) 2_655
B1 F3 1.294(6) .
B1 F1 1.332(6) .
B1 F4 1.356(5) .
B1 F2 1.360(6) .
