#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:42:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179512 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/09/4340997.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_4340997
loop_
_publ_author_name
'Kulmaczewski, Rafal'
'Shepherd, Helena J.'
'Cespedes, Oscar'
'Halcrow, Malcolm A.'
_publ_section_title
;
 A homologous series of [Fe(H₂Bpz₂)₂(L)]
 spin-crossover complexes with annelated bipyridyl co-ligands.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9809
_journal_page_last               9817
_journal_paper_doi               10.1021/ic501402q
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C26 H24 B2 Fe N12, 2[C14 H8 N4]'
_chemical_formula_sum            'C54 H40 B2 Fe N20'
_chemical_formula_weight         1046.53
_chemical_name_systematic
; 
Bis[di(pyrazol-1-yl)dihydridoborate][1,4,8,9-tetraaza-triphenylene]-
iron(II) di-[1,4,8,9-tetraaza-triphenylene] solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 119.592(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.1535(13)
_cell_length_b                   13.8310(6)
_cell_length_c                   14.9300(7)
_cell_measurement_reflns_used    4135
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.62
_cell_volume                     4696.2(4)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.849
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13446
_diffrn_reflns_theta_full        29.67
_diffrn_reflns_theta_max         29.67
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0623
_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)+(0.0678P)²+2.1133P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1577
_reflns_number_gt                4096
_reflns_number_total             5649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501402q_si_003.cif
_cod_data_source_block           rk14a100
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4340990--4341018.cif.
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4340997
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.25887(3) 0.2500 0.01321(16) Uani 1 2 d S
N3 N -0.12127(9) 0.29898(15) 0.07464(17) 0.0170(5) Uani 1 1 d .
N4 N -0.06689(9) 0.26182(14) 0.10352(17) 0.0145(5) Uani 1 1 d .
N8 N -0.09731(9) 0.38425(15) 0.23942(17) 0.0159(5) Uani 1 1 d .
N9 N -0.03830(9) 0.36353(15) 0.28908(16) 0.0145(4) Uani 1 1 d .
N13 N -0.03339(9) 0.15024(15) 0.29158(17) 0.0142(4) Uani 1 1 d .
N20 N -0.03474(9) -0.19999(15) 0.29799(18) 0.0197(5) Uani 1 1 d .
C5 C -0.06576(12) 0.24672(18) 0.0156(2) 0.0171(6) Uani 1 1 d .
H5 H -0.0330 0.2213 0.0123 0.020 Uiso 1 1 calc R
C6 C -0.11861(12) 0.27298(19) -0.0697(2) 0.0208(6) Uani 1 1 d .
H6 H -0.1290 0.2694 -0.1403 0.025 Uiso 1 1 calc R
C7 C -0.15250(12) 0.3055(2) -0.0286(2) 0.0224(6) Uani 1 1 d .
H7 H -0.1917 0.3287 -0.0671 0.027 Uiso 1 1 calc R
C10 C -0.01219(12) 0.43230(18) 0.3601(2) 0.0182(6) Uani 1 1 d .
H10 H 0.0290 0.4363 0.4057 0.022 Uiso 1 1 calc R
C11 C -0.05338(12) 0.49789(18) 0.3588(2) 0.0198(6) Uani 1 1 d .
H11 H -0.0464 0.5527 0.4017 0.024 Uiso 1 1 calc R
C12 C -0.10630(12) 0.46443(18) 0.2810(2) 0.0198(6) Uani 1 1 d .
H12 H -0.1435 0.4934 0.2599 0.024 Uiso 1 1 calc R
C14 C -0.01786(10) 0.06101(17) 0.2743(2) 0.0139(5) Uani 1 1 d .
C15 C -0.03449(11) -0.02574(18) 0.3010(2) 0.0155(5) Uani 1 1 d .
C16 C -0.06677(11) -0.01960(19) 0.3530(2) 0.0187(6) Uani 1 1 d .
H16 H -0.0785 -0.0766 0.3736 0.022 Uiso 1 1 calc R
C17 C -0.08125(12) 0.06992(19) 0.3738(2) 0.0210(6) Uani 1 1 d .
H17 H -0.1024 0.0754 0.4101 0.025 Uiso 1 1 calc R
C18 C -0.06463(11) 0.15239(19) 0.3412(2) 0.0177(6) Uani 1 1 d .
H18 H -0.0759 0.2136 0.3547 0.021 Uiso 1 1 calc R
C19 C -0.01705(11) -0.11651(18) 0.2745(2) 0.0165(5) Uani 1 1 d .
C21 C -0.01763(12) -0.28079(18) 0.2733(2) 0.0217(6) Uani 1 1 d .
H21 H -0.0296 -0.3409 0.2877 0.026 Uiso 1 1 calc R
B2 B -0.14361(13) 0.3203(2) 0.1516(2) 0.0193(6) Uani 1 1 d .
H2A H -0.1819 0.3543 0.1160 0.023 Uiso 1 1 calc R
H2B H -0.1491 0.2590 0.1802 0.023 Uiso 1 1 calc R
N22 N -0.10880(10) -0.24283(15) 0.00614(18) 0.0179(5) Uani 1 1 d .
N28 N -0.13567(10) -0.05766(16) 0.03169(19) 0.0217(5) Uani 1 1 d .
N36 N -0.24562(10) -0.17478(19) 0.19131(19) 0.0274(6) Uani 1 1 d .
N39 N -0.22194(9) -0.36641(18) 0.15733(18) 0.0239(5) Uani 1 1 d .
C23 C -0.14279(11) -0.23004(19) 0.0505(2) 0.0166(5) Uani 1 1 d .
C24 C -0.16559(11) -0.30807(19) 0.0806(2) 0.0176(6) Uani 1 1 d .
C25 C -0.15485(12) -0.40207(19) 0.0592(2) 0.0205(6) Uani 1 1 d .
H25 H -0.1703 -0.4562 0.0772 0.025 Uiso 1 1 calc R
C26 C -0.12192(11) -0.41494(19) 0.0121(2) 0.0217(6) Uani 1 1 d .
H26 H -0.1147 -0.4779 -0.0044 0.026 Uiso 1 1 calc R
C27 C -0.09910(11) -0.33322(19) -0.0111(2) 0.0206(6) Uani 1 1 d .
H27 H -0.0750 -0.3432 -0.0414 0.025 Uiso 1 1 calc R
C29 C -0.15640(11) -0.13006(19) 0.0659(2) 0.0167(5) Uani 1 1 d .
C30 C -0.19170(11) -0.11386(19) 0.1113(2) 0.0192(6) Uani 1 1 d .
C31 C -0.20661(12) -0.0175(2) 0.1189(2) 0.0256(7) Uani 1 1 d .
H31 H -0.2303 -0.0034 0.1492 0.031 Uiso 1 1 calc R
C32 C -0.18678(13) 0.0553(2) 0.0824(3) 0.0283(7) Uani 1 1 d .
H32 H -0.1972 0.1206 0.0853 0.034 Uiso 1 1 calc R
C33 C -0.15079(12) 0.0322(2) 0.0407(2) 0.0254(7) Uani 1 1 d .
H33 H -0.1363 0.0837 0.0173 0.030 Uiso 1 1 calc R
C34 C -0.20070(11) -0.2895(2) 0.1300(2) 0.0198(6) Uani 1 1 d .
C35 C -0.21293(11) -0.1941(2) 0.1459(2) 0.0206(6) Uani 1 1 d .
C37 C -0.26615(13) -0.2504(2) 0.2170(2) 0.0312(8) Uani 1 1 d .
H37 H -0.2896 -0.2398 0.2486 0.037 Uiso 1 1 calc R
C38 C -0.25505(12) -0.3455(2) 0.2000(2) 0.0300(7) Uani 1 1 d .
H38 H -0.2716 -0.3970 0.2194 0.036 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'
B B 0.0013 0.0007 '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'
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'
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
N13 Fe1 N13 81.62(12) . 2
N13 Fe1 N9 95.47(8) . .
N13 Fe1 N9 176.39(8) . 2
N9 Fe1 N9 87.51(11) . 2
N13 Fe1 N4 87.49(9) . 2
N9 Fe1 N4 87.72(8) . 2
N13 Fe1 N4 94.27(9) . .
N9 Fe1 N4 90.60(8) . .
N4 Fe1 N4 177.68(12) 2 .
C7 N3 N4 109.6(2) . .
C7 N3 B2 126.7(2) . .
N4 N3 B2 123.4(2) . .
C5 N4 N3 105.8(2) . .
C5 N4 Fe1 129.09(18) . .
N3 N4 Fe1 124.07(17) . .
C12 N8 N9 109.2(2) . .
C12 N8 B2 128.2(2) . .
N9 N8 B2 122.6(2) . .
C10 N9 N8 106.1(2) . .
C10 N9 Fe1 127.81(17) . .
N8 N9 Fe1 125.73(16) . .
C18 N13 C14 116.2(2) . .
C18 N13 Fe1 129.43(18) . .
C14 N13 Fe1 114.08(16) . .
C21 N20 C19 116.3(2) . .
N4 C5 C6 111.3(2) . .
N4 C5 H5 124.3 . .
C6 C5 H5 124.3 . .
C7 C6 C5 104.1(2) . .
C7 C6 H6 127.9 . .
C5 C6 H6 127.9 . .
N3 C7 C6 109.2(2) . .
N3 C7 H7 125.4 . .
C6 C7 H7 125.4 . .
N9 C10 C11 111.2(2) . .
N9 C10 H10 124.4 . .
C11 C10 H10 124.4 . .
C12 C11 C10 103.9(2) . .
C12 C11 H11 128.0 . .
C10 C11 H11 128.0 . .
N8 C12 C11 109.5(2) . .
N8 C12 H12 125.2 . .
C11 C12 H12 125.2 . .
N13 C14 C15 124.0(2) . .
N13 C14 C14 115.07(13) . 2
C15 C14 C14 120.94(14) . 2
C14 C15 C16 117.5(2) . .
C14 C15 C19 118.6(2) . .
C16 C15 C19 123.9(2) . .
C17 C16 C15 119.2(2) . .
C17 C16 H16 120.4 . .
C15 C16 H16 120.4 . .
C16 C17 C18 119.4(2) . .
C16 C17 H17 120.3 . .
C18 C17 H17 120.3 . .
N13 C18 C17 123.6(2) . .
N13 C18 H18 118.2 . .
C17 C18 H18 118.2 . .
N20 C19 C19 121.41(14) . 2
N20 C19 C15 118.2(2) . .
C19 C19 C15 120.41(14) 2 .
N20 C21 C21 122.27(15) . 2
N20 C21 H21 118.9 . .
C21 C21 H21 118.9 2 .
N8 B2 N3 108.2(2) . .
N8 B2 H2A 110.1 . .
N3 B2 H2A 110.1 . .
N8 B2 H2B 110.1 . .
N3 B2 H2B 110.1 . .
H2A B2 H2B 108.4 . .
C27 N22 C23 116.9(2) . .
C33 N28 C29 117.3(2) . .
C37 N36 C35 116.0(3) . .
C38 N39 C34 115.7(3) . .
N22 C23 C24 122.5(2) . .
N22 C23 C29 117.7(2) . .
C24 C23 C29 119.8(2) . .
C25 C24 C23 118.4(2) . .
C25 C24 C34 121.8(2) . .
C23 C24 C34 119.9(2) . .
C26 C25 C24 119.1(2) . .
C26 C25 H25 120.4 . .
C24 C25 H25 120.4 . .
C25 C26 C27 118.5(2) . .
C25 C26 H26 120.7 . .
C27 C26 H26 120.7 . .
N22 C27 C26 124.5(2) . .
N22 C27 H27 117.7 . .
C26 C27 H27 117.7 . .
N28 C29 C30 123.0(2) . .
N28 C29 C23 117.6(2) . .
C30 C29 C23 119.4(2) . .
C29 C30 C31 117.6(3) . .
C29 C30 C35 120.6(2) . .
C31 C30 C35 121.8(2) . .
C32 C31 C30 119.5(3) . .
C32 C31 H31 120.3 . .
C30 C31 H31 120.3 . .
C31 C32 C33 118.8(3) . .
C31 C32 H32 120.6 . .
C33 C32 H32 120.6 . .
N28 C33 C32 123.8(3) . .
N28 C33 H33 118.1 . .
C32 C33 H33 118.1 . .
N39 C34 C35 121.7(2) . .
N39 C34 C24 118.0(2) . .
C35 C34 C24 120.2(2) . .
N36 C35 C34 121.5(3) . .
N36 C35 C30 118.4(3) . .
C34 C35 C30 120.1(2) . .
N36 C37 C38 122.9(3) . .
N36 C37 H37 118.5 . .
C38 C37 H37 118.5 . .
N39 C38 C37 122.2(3) . .
N39 C38 H38 118.9 . .
C37 C38 H38 118.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N13 1.985(2) .
Fe1 N9 2.004(2) .
Fe1 N4 2.017(2) .
N3 C7 1.344(4) .
N3 N4 1.367(3) .
N3 B2 1.553(4) .
N4 C5 1.343(3) .
N8 C12 1.347(3) .
N8 N9 1.373(3) .
N8 B2 1.549(4) .
N9 C10 1.335(3) .
N13 C18 1.348(3) .
N13 C14 1.363(3) .
N20 C21 1.322(3) .
N20 C19 1.353(3) .
C5 C6 1.388(4) .
C5 H5 0.9500 .
C6 C7 1.379(4) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C10 C11 1.401(4) .
C10 H10 0.9500 .
C11 C12 1.375(4) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C14 C15 1.400(3) .
C14 C14 1.439(5) 2
C15 C16 1.404(4) .
C15 C19 1.456(3) .
C16 C17 1.374(4) .
C16 H16 0.9500 .
C17 C18 1.391(4) .
C17 H17 0.9500 .
C18 H18 0.9500 .
C19 C19 1.405(5) 2
C21 C21 1.404(6) 2
C21 H21 0.9500 .
B2 H2A 0.9900 .
B2 H2B 0.9900 .
N22 C27 1.326(3) .
N22 C23 1.358(3) .
N28 C33 1.331(3) .
N28 C29 1.353(3) .
N36 C37 1.317(4) .
N36 C35 1.354(3) .
N39 C38 1.335(4) .
N39 C34 1.352(3) .
C23 C24 1.409(4) .
C23 C29 1.474(4) .
C24 C25 1.400(4) .
C24 C34 1.457(4) .
C25 C26 1.366(4) .
C25 H25 0.9500 .
C26 C27 1.400(4) .
C26 H26 0.9500 .
C27 H27 0.9500 .
C29 C30 1.408(4) .
C30 C31 1.408(4) .
C30 C35 1.445(4) .
C31 C32 1.364(4) .
C31 H31 0.9500 .
C32 C33 1.399(4) .
C32 H32 0.9500 .
C33 H33 0.9500 .
C34 C35 1.405(4) .
C37 C38 1.397(5) .
C37 H37 0.9500 .
C38 H38 0.9500 .
