#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:46:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179513 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/10/4341001.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_4341001
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                 119.063(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.2962(18)
_cell_length_b                   13.9778(7)
_cell_length_c                   14.9991(9)
_cell_measurement_reflns_used    3471
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.00
_cell_volume                     4818.9(6)
_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      180(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.850
_diffrn_measured_fraction_theta_max 0.850
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0809
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13910
_diffrn_reflns_theta_full        29.70
_diffrn_reflns_theta_max         29.70
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.875
_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    1.442
_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         0.889
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0633
_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)+(0.0656P)²+0.1339P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                3864
_reflns_number_total             5822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501402q_si_003.cif
_cod_data_source_block           rk14a180
_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_cell_volume        4818.9(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4341001
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 0.26295(4) 0.2500 0.02149(17) Uani 1 2 d S
N3 N -0.12611(9) 0.30337(17) 0.07211(19) 0.0295(6) Uani 1 1 d .
N4 N -0.07240(9) 0.26902(16) 0.09653(19) 0.0281(5) Uani 1 1 d .
N8 N -0.10212(9) 0.38653(15) 0.23868(18) 0.0278(5) Uani 1 1 d .
N9 N -0.04383(9) 0.36847(15) 0.29091(18) 0.0271(5) Uani 1 1 d .
N13 N -0.03091(9) 0.13876(15) 0.29922(17) 0.0244(5) Uani 1 1 d .
N20 N -0.03352(10) -0.20639(16) 0.2998(2) 0.0332(6) Uani 1 1 d .
C5 C -0.07265(13) 0.25766(19) 0.0080(2) 0.0319(7) Uani 1 1 d .
H5 H -0.0404 0.2348 0.0020 0.038 Uiso 1 1 calc R
C6 C -0.12573(13) 0.2833(2) -0.0740(2) 0.0385(8) Uani 1 1 d .
H6 H -0.1370 0.2816 -0.1446 0.046 Uiso 1 1 calc R
C7 C -0.15817(13) 0.3117(2) -0.0291(2) 0.0406(8) Uani 1 1 d .
H7 H -0.1972 0.3338 -0.0646 0.049 Uiso 1 1 calc R
C10 C -0.02043(13) 0.43823(19) 0.3599(2) 0.0329(7) Uani 1 1 d .
H10 H 0.0199 0.4440 0.4067 0.039 Uiso 1 1 calc R
C11 C -0.06266(14) 0.5014(2) 0.3544(2) 0.0384(8) Uani 1 1 d .
H11 H -0.0574 0.5564 0.3951 0.046 Uiso 1 1 calc R
C12 C -0.11351(14) 0.4661(2) 0.2769(2) 0.0360(7) Uani 1 1 d .
H12 H -0.1510 0.4933 0.2537 0.043 Uiso 1 1 calc R
C14 C -0.01660(10) 0.05227(18) 0.2775(2) 0.0223(6) Uani 1 1 d .
C15 C -0.03225(11) -0.03383(19) 0.3043(2) 0.0250(6) Uani 1 1 d .
C16 C -0.06304(11) -0.0292(2) 0.3591(2) 0.0316(7) Uani 1 1 d .
H16 H -0.0743 -0.0863 0.3792 0.038 Uiso 1 1 calc R
C17 C -0.07655(12) 0.0581(2) 0.3831(2) 0.0332(7) Uani 1 1 d .
H17 H -0.0968 0.0626 0.4210 0.040 Uiso 1 1 calc R
C18 C -0.06015(11) 0.1404(2) 0.3511(2) 0.0286(6) Uani 1 1 d .
H18 H -0.0703 0.2007 0.3670 0.034 Uiso 1 1 calc R
C19 C -0.01606(11) -0.12412(18) 0.2759(2) 0.0265(6) Uani 1 1 d .
C21 C -0.01712(13) -0.2861(2) 0.2739(3) 0.0393(8) Uani 1 1 d .
H21 H -0.0291 -0.3456 0.2882 0.047 Uiso 1 1 calc R
B2 B -0.14540(14) 0.3186(2) 0.1541(3) 0.0318(8) Uani 1 1 d .
H2A H -0.1850 0.3466 0.1218 0.038 Uiso 1 1 calc R
H2B H -0.1466 0.2563 0.1844 0.038 Uiso 1 1 calc R
N22 N -0.10845(10) -0.24145(15) 0.0092(2) 0.0290(6) Uani 1 1 d .
N28 N -0.13399(10) -0.05851(16) 0.0381(2) 0.0344(6) Uani 1 1 d .
N36 N -0.24718(10) -0.1764(2) 0.1896(2) 0.0414(7) Uani 1 1 d .
N39 N -0.22455(10) -0.36552(18) 0.1526(2) 0.0353(6) Uani 1 1 d .
C23 C -0.14254(11) -0.22899(19) 0.0528(2) 0.0243(6) Uani 1 1 d .
C24 C -0.16601(11) -0.30665(19) 0.0805(2) 0.0251(6) Uani 1 1 d .
C25 C -0.15510(12) -0.3996(2) 0.0593(2) 0.0309(7) Uani 1 1 d .
H25 H -0.1709 -0.4534 0.0762 0.037 Uiso 1 1 calc R
C26 C -0.12132(12) -0.4117(2) 0.0138(2) 0.0343(7) Uani 1 1 d .
H26 H -0.1134 -0.4738 -0.0020 0.041 Uiso 1 1 calc R
C27 C -0.09876(12) -0.3308(2) -0.0087(2) 0.0335(7) Uani 1 1 d .
H27 H -0.0747 -0.3402 -0.0391 0.040 Uiso 1 1 calc R
C29 C -0.15553(11) -0.13049(18) 0.0696(2) 0.0249(6) Uani 1 1 d .
C30 C -0.19116(11) -0.1147(2) 0.1142(2) 0.0294(6) Uani 1 1 d .
C31 C -0.20529(12) -0.0204(2) 0.1238(3) 0.0402(8) Uani 1 1 d .
H31 H -0.2295 -0.0070 0.1528 0.048 Uiso 1 1 calc R
C32 C -0.18408(14) 0.0523(2) 0.0911(3) 0.0464(9) Uani 1 1 d .
H32 H -0.1935 0.1169 0.0966 0.056 Uiso 1 1 calc R
C33 C -0.14814(13) 0.0300(2) 0.0493(3) 0.0422(8) Uani 1 1 d .
H33 H -0.1330 0.0813 0.0276 0.051 Uiso 1 1 calc R
C34 C -0.20215(11) -0.2894(2) 0.1282(2) 0.0269(6) Uani 1 1 d .
C35 C -0.21386(11) -0.1954(2) 0.1454(2) 0.0296(6) Uani 1 1 d .
C37 C -0.26899(14) -0.2517(3) 0.2122(3) 0.0465(9) Uani 1 1 d .
H37 H -0.2930 -0.2417 0.2425 0.056 Uiso 1 1 calc R
C38 C -0.25832(12) -0.3451(3) 0.1935(3) 0.0455(9) Uani 1 1 d .
H38 H -0.2758 -0.3963 0.2105 0.055 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
N9 Fe1 N9 92.72(11) 2 .
N9 Fe1 N4 87.69(9) . .
N9 Fe1 N4 89.20(9) . 2
N4 Fe1 N4 175.50(12) . 2
N9 Fe1 N13 96.31(8) . .
N4 Fe1 N13 96.37(8) . .
N9 Fe1 N13 169.56(8) . 2
N4 Fe1 N13 87.21(8) . 2
N13 Fe1 N13 75.22(11) . 2
C7 N3 N4 109.6(2) . .
C7 N3 B2 128.2(2) . .
N4 N3 B2 122.0(2) . .
C5 N4 N3 105.7(2) . .
C5 N4 Fe1 129.13(19) . .
N3 N4 Fe1 124.17(18) . .
C12 N8 N9 109.1(2) . .
C12 N8 B2 128.8(2) . .
N9 N8 B2 122.0(2) . .
C10 N9 N8 106.0(2) . .
C10 N9 Fe1 128.08(19) . .
N8 N9 Fe1 125.11(17) . .
C18 N13 C14 117.6(2) . .
C18 N13 Fe1 126.61(18) . .
C14 N13 Fe1 115.78(16) . .
C21 N20 C19 116.0(3) . .
N4 C5 C6 111.6(3) . .
N4 C5 H5 124.2 . .
C6 C5 H5 124.2 . .
C7 C6 C5 103.7(3) . .
C7 C6 H6 128.2 . .
C5 C6 H6 128.2 . .
N3 C7 C6 109.4(3) . .
N3 C7 H7 125.3 . .
C6 C7 H7 125.3 . .
N9 C10 C11 111.3(3) . .
N9 C10 H10 124.3 . .
C11 C10 H10 124.3 . .
C12 C11 C10 104.2(3) . .
C12 C11 H11 127.9 . .
C10 C11 H11 127.9 . .
N8 C12 C11 109.3(3) . .
N8 C12 H12 125.3 . .
C11 C12 H12 125.3 . .
N13 C14 C15 123.2(2) . .
N13 C14 C14 116.61(14) . 2
C15 C14 C14 120.23(15) . 2
C14 C15 C16 117.6(2) . .
C14 C15 C19 119.6(2) . .
C16 C15 C19 122.8(2) . .
C17 C16 C15 119.4(3) . .
C17 C16 H16 120.3 . .
C15 C16 H16 120.3 . .
C16 C17 C18 118.8(3) . .
C16 C17 H17 120.6 . .
C18 C17 H17 120.6 . .
N13 C18 C17 123.4(3) . .
N13 C18 H18 118.3 . .
C17 C18 H18 118.3 . .
N20 C19 C19 121.51(16) . 2
N20 C19 C15 118.3(2) . .
C19 C19 C15 120.15(14) 2 .
N20 C21 C21 122.40(17) . 2
N20 C21 H21 118.8 . .
C21 C21 H21 118.8 2 .
N8 B2 N3 109.8(2) . .
N8 B2 H2A 109.7 . .
N3 B2 H2A 109.7 . .
N8 B2 H2B 109.7 . .
N3 B2 H2B 109.7 . .
H2A B2 H2B 108.2 . .
C27 N22 C23 117.2(2) . .
C33 N28 C29 117.5(3) . .
C37 N36 C35 115.7(3) . .
C38 N39 C34 115.6(3) . .
N22 C23 C24 122.1(2) . .
N22 C23 C29 117.8(2) . .
C24 C23 C29 120.0(2) . .
C25 C24 C23 118.8(2) . .
C25 C24 C34 121.2(2) . .
C23 C24 C34 120.0(2) . .
C26 C25 C24 118.8(3) . .
C26 C25 H25 120.6 . .
C24 C25 H25 120.6 . .
C25 C26 C27 118.5(3) . .
C25 C26 H26 120.7 . .
C27 C26 H26 120.7 . .
N22 C27 C26 124.6(3) . .
N22 C27 H27 117.7 . .
C26 C27 H27 117.7 . .
N28 C29 C30 122.7(2) . .
N28 C29 C23 117.9(2) . .
C30 C29 C23 119.4(2) . .
C31 C30 C29 117.9(3) . .
C31 C30 C35 121.9(3) . .
C29 C30 C35 120.2(2) . .
C32 C31 C30 119.5(3) . .
C32 C31 H31 120.2 . .
C30 C31 H31 120.2 . .
C31 C32 C33 118.7(3) . .
C31 C32 H32 120.7 . .
C33 C32 H32 120.7 . .
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 118.4(3) . .
C35 C34 C24 119.9(3) . .
N36 C35 C34 121.7(3) . .
N36 C35 C30 117.9(3) . .
C34 C35 C30 120.4(2) . .
N36 C37 C38 122.8(3) . .
N36 C37 H37 118.6 . .
C38 C37 H37 118.6 . .
N39 C38 C37 122.6(3) . .
N39 C38 H38 118.7 . .
C37 C38 H38 118.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N9 2.137(2) .
Fe1 N4 2.162(2) .
Fe1 N13 2.191(2) .
N3 C7 1.337(4) .
N3 N4 1.363(3) .
N3 B2 1.555(4) .
N4 C5 1.334(4) .
N8 C12 1.350(3) .
N8 N9 1.364(3) .
N8 B2 1.550(4) .
N9 C10 1.334(3) .
N13 C18 1.333(3) .
N13 C14 1.352(3) .
N20 C21 1.320(4) .
N20 C19 1.350(3) .
C5 C6 1.386(4) .
C5 H5 0.9500 .
C6 C7 1.377(4) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C10 C11 1.389(4) .
C10 H10 0.9500 .
C11 C12 1.368(4) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C14 C15 1.393(3) .
C14 C14 1.463(5) 2
C15 C16 1.408(4) .
C15 C19 1.460(4) .
C16 C17 1.368(4) .
C16 H16 0.9500 .
C17 C18 1.393(4) .
C17 H17 0.9500 .
C18 H18 0.9500 .
C19 C19 1.399(5) 2
C21 C21 1.396(6) 2
C21 H21 0.9500 .
B2 H2A 0.9900 .
B2 H2B 0.9900 .
N22 C27 1.328(3) .
N22 C23 1.353(3) .
N28 C33 1.326(4) .
N28 C29 1.347(3) .
N36 C37 1.319(4) .
N36 C35 1.358(3) .
N39 C38 1.332(4) .
N39 C34 1.350(3) .
C23 C24 1.407(4) .
C23 C29 1.469(4) .
C24 C25 1.400(4) .
C24 C34 1.461(4) .
C25 C26 1.368(4) .
C25 H25 0.9500 .
C26 C27 1.393(4) .
C26 H26 0.9500 .
C27 H27 0.9500 .
C29 C30 1.409(4) .
C30 C31 1.397(4) .
C30 C35 1.455(4) .
C31 C32 1.359(4) .
C31 H31 0.9500 .
C32 C33 1.400(4) .
C32 H32 0.9500 .
C33 H33 0.9500 .
C34 C35 1.400(4) .
C37 C38 1.393(5) .
C37 H37 0.9500 .
C38 H38 0.9500 .
