#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:46:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179513 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/10/4341004.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_4341004
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                 118.858(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.3433(19)
_cell_length_b                   14.0332(8)
_cell_length_c                   15.0438(11)
_cell_measurement_reflns_used    2958
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      1.99
_cell_volume                     4870.8(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      240(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.843
_diffrn_measured_fraction_theta_max 0.843
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0863
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -36
_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            14094
_diffrn_reflns_theta_full        29.80
_diffrn_reflns_theta_max         29.80
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.889
_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    1.427
_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         0.772
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0660
_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)+(0.0622P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1636
_reflns_number_gt                3513
_reflns_number_total             5883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501402q_si_003.cif
_cod_data_source_block           rk14a240
_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               4341004
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 0.26289(4) 0.2500 0.02813(19) Uani 1 2 d S
N3 N -0.12634(10) 0.30335(18) 0.0727(2) 0.0382(6) Uani 1 1 d .
N4 N -0.07299(10) 0.26910(17) 0.0960(2) 0.0341(6) Uani 1 1 d .
N8 N -0.10247(10) 0.38631(16) 0.2386(2) 0.0352(6) Uani 1 1 d .
N9 N -0.04447(10) 0.36846(16) 0.2910(2) 0.0349(6) Uani 1 1 d .
N13 N -0.03069(9) 0.13690(16) 0.29982(19) 0.0307(6) Uani 1 1 d .
N20 N -0.03335(11) -0.20698(17) 0.3001(2) 0.0447(7) Uani 1 1 d .
C5 C -0.07319(14) 0.2579(2) 0.0076(3) 0.0399(8) Uani 1 1 d .
H5 H -0.0415 0.2352 0.0012 0.048 Uiso 1 1 calc R
C6 C -0.12590(14) 0.2841(2) -0.0732(3) 0.0482(9) Uani 1 1 d .
H6 H -0.1372 0.2828 -0.1428 0.058 Uiso 1 1 calc R
C7 C -0.15792(14) 0.3125(3) -0.0281(3) 0.0523(9) Uani 1 1 d .
H7 H -0.1963 0.3351 -0.0628 0.063 Uiso 1 1 calc R
C10 C -0.02150(14) 0.4381(2) 0.3589(3) 0.0409(8) Uani 1 1 d .
H10 H 0.0183 0.4440 0.4050 0.049 Uiso 1 1 calc R
C11 C -0.06349(16) 0.5006(2) 0.3532(3) 0.0479(9) Uani 1 1 d .
H11 H -0.0585 0.5550 0.3931 0.057 Uiso 1 1 calc R
C12 C -0.11410(16) 0.4653(2) 0.2761(3) 0.0472(9) Uani 1 1 d .
H12 H -0.1511 0.4920 0.2531 0.057 Uiso 1 1 calc R
C14 C -0.01648(11) 0.05109(18) 0.2777(2) 0.0270(6) Uani 1 1 d .
C15 C -0.03202(11) -0.03480(19) 0.3048(2) 0.0316(7) Uani 1 1 d .
C16 C -0.06235(12) -0.0305(2) 0.3598(3) 0.0380(8) Uani 1 1 d .
H16 H -0.0733 -0.0868 0.3799 0.046 Uiso 1 1 calc R
C17 C -0.07596(13) 0.0565(2) 0.3839(3) 0.0410(8) Uani 1 1 d .
H17 H -0.0959 0.0609 0.4213 0.049 Uiso 1 1 calc R
C18 C -0.05969(12) 0.1380(2) 0.3519(2) 0.0368(7) Uani 1 1 d .
H18 H -0.0697 0.1975 0.3678 0.044 Uiso 1 1 calc R
C19 C -0.01610(12) -0.12484(19) 0.2762(2) 0.0337(7) Uani 1 1 d .
C21 C -0.01701(14) -0.2860(2) 0.2741(3) 0.0513(9) Uani 1 1 d .
H21 H -0.0286 -0.3447 0.2885 0.062 Uiso 1 1 calc R
B2 B -0.14516(15) 0.3183(3) 0.1546(3) 0.0428(9) Uani 1 1 d .
H2A H -0.1843 0.3454 0.1232 0.051 Uiso 1 1 calc R
H2B H -0.1460 0.2568 0.1847 0.051 Uiso 1 1 calc R
N22 N -0.10868(11) -0.24046(17) 0.0090(2) 0.0392(6) Uani 1 1 d .
N28 N -0.13380(11) -0.05882(18) 0.0387(2) 0.0453(7) Uani 1 1 d .
N36 N -0.24706(12) -0.1768(2) 0.1892(2) 0.0562(8) Uani 1 1 d .
N39 N -0.22461(11) -0.3648(2) 0.1522(2) 0.0475(7) Uani 1 1 d .
C23 C -0.14264(11) -0.2287(2) 0.0533(2) 0.0323(7) Uani 1 1 d .
C24 C -0.16588(11) -0.3057(2) 0.0807(2) 0.0331(7) Uani 1 1 d .
C25 C -0.15479(13) -0.3983(2) 0.0599(3) 0.0406(8) Uani 1 1 d .
H25 H -0.1702 -0.4514 0.0768 0.049 Uiso 1 1 calc R
C26 C -0.12113(14) -0.4100(2) 0.0147(3) 0.0476(9) Uani 1 1 d .
H26 H -0.1131 -0.4712 -0.0007 0.057 Uiso 1 1 calc R
C27 C -0.09886(13) -0.3295(2) -0.0082(3) 0.0451(8) Uani 1 1 d .
H27 H -0.0751 -0.3389 -0.0381 0.054 Uiso 1 1 calc R
C29 C -0.15576(12) -0.1305(2) 0.0696(2) 0.0338(7) Uani 1 1 d .
C30 C -0.19099(12) -0.1147(2) 0.1146(2) 0.0374(7) Uani 1 1 d .
C31 C -0.20492(14) -0.0207(2) 0.1247(3) 0.0524(10) Uani 1 1 d .
H31 H -0.2286 -0.0074 0.1539 0.063 Uiso 1 1 calc R
C32 C -0.18370(16) 0.0515(3) 0.0915(3) 0.0628(11) Uani 1 1 d .
H32 H -0.1931 0.1152 0.0965 0.075 Uiso 1 1 calc R
C33 C -0.14792(15) 0.0293(2) 0.0501(3) 0.0540(10) Uani 1 1 d .
H33 H -0.1329 0.0799 0.0290 0.065 Uiso 1 1 calc R
C34 C -0.20199(12) -0.2883(2) 0.1282(2) 0.0371(7) Uani 1 1 d .
C35 C -0.21371(12) -0.1949(2) 0.1454(2) 0.0399(8) Uani 1 1 d .
C37 C -0.26867(15) -0.2513(3) 0.2121(3) 0.0617(11) Uani 1 1 d .
H37 H -0.2922 -0.2415 0.2423 0.074 Uiso 1 1 calc R
C38 C -0.25805(14) -0.3441(3) 0.1933(3) 0.0595(11) Uani 1 1 d .
H38 H -0.2753 -0.3945 0.2104 0.071 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 93.16(12) 2 .
N9 Fe1 N4 89.47(9) . 2
N9 Fe1 N4 87.38(9) . .
N4 Fe1 N4 175.43(13) 2 .
N9 Fe1 N13 168.84(8) . 2
N4 Fe1 N13 87.21(9) . 2
N9 Fe1 N13 96.54(9) . .
N4 Fe1 N13 96.44(9) . .
N13 Fe1 N13 74.39(11) 2 .
C7 N3 N4 109.0(3) . .
C7 N3 B2 128.8(3) . .
N4 N3 B2 122.0(3) . .
C5 N4 N3 106.1(3) . .
C5 N4 Fe1 129.0(2) . .
N3 N4 Fe1 123.9(2) . .
C12 N8 N9 109.1(3) . .
C12 N8 B2 128.9(3) . .
N9 N8 B2 121.9(2) . .
C10 N9 N8 106.1(2) . .
C10 N9 Fe1 128.0(2) . .
N8 N9 Fe1 124.98(18) . .
C18 N13 C14 117.5(2) . .
C18 N13 Fe1 126.49(19) . .
C14 N13 Fe1 115.99(17) . .
C21 N20 C19 116.1(3) . .
N4 C5 C6 111.4(3) . .
N4 C5 H5 124.3 . .
C6 C5 H5 124.3 . .
C7 C6 C5 103.8(3) . .
C7 C6 H6 128.1 . .
C5 C6 H6 128.1 . .
N3 C7 C6 109.8(3) . .
N3 C7 H7 125.1 . .
C6 C7 H7 125.1 . .
N9 C10 C11 111.4(3) . .
N9 C10 H10 124.3 . .
C11 C10 H10 124.3 . .
C12 C11 C10 104.3(3) . .
C12 C11 H11 127.9 . .
C10 C11 H11 127.9 . .
N8 C12 C11 109.1(3) . .
N8 C12 H12 125.4 . .
C11 C12 H12 125.4 . .
N13 C14 C15 122.9(3) . .
N13 C14 C14 116.81(15) . 2
C15 C14 C14 120.25(16) . 2
C14 C15 C16 117.8(3) . .
C14 C15 C19 119.7(3) . .
C16 C15 C19 122.6(3) . .
C17 C16 C15 119.4(3) . .
C17 C16 H16 120.3 . .
C15 C16 H16 120.3 . .
C16 C17 C18 118.6(3) . .
C16 C17 H17 120.7 . .
C18 C17 H17 120.7 . .
N13 C18 C17 123.7(3) . .
N13 C18 H18 118.1 . .
C17 C18 H18 118.1 . .
N20 C19 C19 121.31(18) . 2
N20 C19 C15 118.6(3) . .
C19 C19 C15 120.07(16) 2 .
N20 C21 C21 122.50(19) . 2
N20 C21 H21 118.7 . .
C21 C21 H21 118.7 2 .
N8 B2 N3 110.3(3) . .
N8 B2 H2A 109.6 . .
N3 B2 H2A 109.6 . .
N8 B2 H2B 109.6 . .
N3 B2 H2B 109.6 . .
H2A B2 H2B 108.1 . .
C27 N22 C23 116.6(3) . .
C33 N28 C29 117.2(3) . .
C37 N36 C35 116.3(3) . .
C38 N39 C34 115.2(3) . .
N22 C23 C24 122.4(3) . .
N22 C23 C29 117.3(3) . .
C24 C23 C29 120.3(3) . .
C23 C24 C25 118.9(3) . .
C23 C24 C34 119.7(3) . .
C25 C24 C34 121.3(3) . .
C26 C25 C24 118.6(3) . .
C26 C25 H25 120.7 . .
C24 C25 H25 120.7 . .
C25 C26 C27 118.7(3) . .
C25 C26 H26 120.7 . .
C27 C26 H26 120.7 . .
N22 C27 C26 124.8(3) . .
N22 C27 H27 117.6 . .
C26 C27 H27 117.6 . .
N28 C29 C30 122.8(3) . .
N28 C29 C23 117.8(3) . .
C30 C29 C23 119.4(3) . .
C31 C30 C29 118.0(3) . .
C31 C30 C35 121.8(3) . .
C29 C30 C35 120.1(3) . .
C32 C31 C30 119.1(3) . .
C32 C31 H31 120.4 . .
C30 C31 H31 120.4 . .
C31 C32 C33 118.9(3) . .
C31 C32 H32 120.5 . .
C33 C32 H32 120.5 . .
N28 C33 C32 124.0(3) . .
N28 C33 H33 118.0 . .
C32 C33 H33 118.0 . .
N39 C34 C35 121.8(3) . .
N39 C34 C24 118.1(3) . .
C35 C34 C24 120.1(3) . .
N36 C35 C34 121.3(3) . .
N36 C35 C30 118.3(3) . .
C34 C35 C30 120.4(3) . .
N36 C37 C38 122.5(3) . .
N36 C37 H37 118.7 . .
C38 C37 H37 118.7 . .
N39 C38 C37 122.9(4) . .
N39 C38 H38 118.6 . .
C37 C38 H38 118.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N9 2.155(2) .
Fe1 N4 2.185(3) .
Fe1 N13 2.219(2) .
N3 C7 1.338(4) .
N3 N4 1.361(3) .
N3 B2 1.549(4) .
N4 C5 1.336(4) .
N8 C12 1.345(4) .
N8 N9 1.362(3) .
N8 B2 1.549(4) .
N9 C10 1.329(4) .
N13 C18 1.332(4) .
N13 C14 1.349(3) .
N20 C21 1.315(4) .
N20 C19 1.350(3) .
C5 C6 1.383(4) .
C5 H5 0.9400 .
C6 C7 1.372(5) .
C6 H6 0.9400 .
C7 H7 0.9400 .
C10 C11 1.382(4) .
C10 H10 0.9400 .
C11 C12 1.369(5) .
C11 H11 0.9400 .
C12 H12 0.9400 .
C14 C15 1.395(4) .
C14 C14 1.466(5) 2
C15 C16 1.401(4) .
C15 C19 1.460(4) .
C16 C17 1.370(4) .
C16 H16 0.9400 .
C17 C18 1.387(4) .
C17 H17 0.9400 .
C18 H18 0.9400 .
C19 C19 1.409(6) 2
C21 C21 1.399(7) 2
C21 H21 0.9400 .
B2 H2A 0.9800 .
B2 H2B 0.9800 .
N22 C27 1.327(4) .
N22 C23 1.359(4) .
N28 C33 1.327(4) .
N28 C29 1.350(4) .
N36 C37 1.314(5) .
N36 C35 1.353(4) .
N39 C38 1.329(4) .
N39 C34 1.358(4) .
C23 C24 1.399(4) .
C23 C29 1.470(4) .
C24 C25 1.400(4) .
C24 C34 1.460(4) .
C25 C26 1.363(4) .
C25 H25 0.9400 .
C26 C27 1.391(4) .
C26 H26 0.9400 .
C27 H27 0.9400 .
C29 C30 1.405(4) .
C30 C31 1.397(4) .
C30 C35 1.452(4) .
C31 C32 1.362(5) .
C31 H31 0.9400 .
C32 C33 1.393(5) .
C32 H32 0.9400 .
C33 H33 0.9400 .
C34 C35 1.399(4) .
C37 C38 1.389(5) .
C37 H37 0.9400 .
C38 H38 0.9400 .
