#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:46:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179513 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/10/4341005.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_4341005
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                 118.775(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.373(2)
_cell_length_b                   14.0601(8)
_cell_length_c                   15.0664(11)
_cell_measurement_reflns_used    2829
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      24.63
_cell_measurement_theta_min      1.99
_cell_volume                     4896.9(7)
_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      260(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.844
_diffrn_measured_fraction_theta_max 0.844
_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  0.0621
_diffrn_reflns_av_sigmaI/netI    0.1011
_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            14125
_diffrn_reflns_theta_full        29.76
_diffrn_reflns_theta_max         29.76
_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    0.371
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.779
_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    1.420
_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         0.764
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1309
_refine_ls_R_factor_gt           0.0705
_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)+(0.0614P)²+2.1265P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1744
_reflns_number_gt                3431
_reflns_number_total             5902
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501402q_si_003.cif
_cod_data_source_block           rk14a260
_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        4896.9(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4341005
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 0.26272(4) 0.2500 0.0303(2) Uani 1 2 d S
N3 N -0.12616(11) 0.3035(2) 0.0730(2) 0.0403(7) Uani 1 1 d .
N4 N -0.07306(11) 0.26903(18) 0.0959(2) 0.0367(7) Uani 1 1 d .
N8 N -0.10245(11) 0.38637(18) 0.2386(2) 0.0377(7) Uani 1 1 d .
N9 N -0.04458(11) 0.36818(17) 0.2909(2) 0.0359(6) Uani 1 1 d .
N13 N -0.03066(10) 0.13652(17) 0.3000(2) 0.0319(6) Uani 1 1 d .
N20 N -0.03304(12) -0.20657(19) 0.3005(2) 0.0469(8) Uani 1 1 d .
C5 C -0.07341(15) 0.2578(2) 0.0077(3) 0.0408(8) Uani 1 1 d .
H5 H -0.0422 0.2349 0.0014 0.049 Uiso 1 1 calc R
C6 C -0.12549(16) 0.2842(3) -0.0727(3) 0.0520(10) Uani 1 1 d .
H6 H -0.1363 0.2831 -0.1413 0.062 Uiso 1 1 calc R
C7 C -0.15791(16) 0.3128(3) -0.0278(3) 0.0576(11) Uani 1 1 d .
H7 H -0.1958 0.3351 -0.0620 0.069 Uiso 1 1 calc R
C10 C -0.02151(16) 0.4381(2) 0.3589(3) 0.0437(9) Uani 1 1 d .
H10 H 0.0178 0.4441 0.4042 0.052 Uiso 1 1 calc R
C11 C -0.06367(18) 0.5005(2) 0.3531(3) 0.0504(10) Uani 1 1 d .
H11 H -0.0588 0.5541 0.3927 0.060 Uiso 1 1 calc R
C12 C -0.11415(18) 0.4654(2) 0.2758(3) 0.0495(10) Uani 1 1 d .
H12 H -0.1507 0.4919 0.2528 0.059 Uiso 1 1 calc R
C14 C -0.01651(12) 0.0507(2) 0.2777(2) 0.0286(7) Uani 1 1 d .
C15 C -0.03188(12) -0.0353(2) 0.3050(2) 0.0330(7) Uani 1 1 d .
C16 C -0.06243(14) -0.0306(2) 0.3595(3) 0.0427(9) Uani 1 1 d .
H16 H -0.0739 -0.0862 0.3783 0.051 Uiso 1 1 calc R
C17 C -0.07545(14) 0.0563(2) 0.3849(3) 0.0448(9) Uani 1 1 d .
H17 H -0.0944 0.0605 0.4232 0.054 Uiso 1 1 calc R
C18 C -0.05960(14) 0.1379(2) 0.3519(3) 0.0393(8) Uani 1 1 d .
H18 H -0.0698 0.1966 0.3670 0.047 Uiso 1 1 calc R
C19 C -0.01595(13) -0.1248(2) 0.2761(3) 0.0358(8) Uani 1 1 d .
C21 C -0.01657(16) -0.2855(2) 0.2747(3) 0.0561(11) Uani 1 1 d .
H21 H -0.0275 -0.3435 0.2900 0.067 Uiso 1 1 calc R
B2 B -0.14515(16) 0.3180(3) 0.1547(3) 0.0468(11) Uani 1 1 d .
H2A H -0.1458 0.2572 0.1844 0.056 Uiso 1 1 calc R
H2B H -0.1839 0.3445 0.1237 0.056 Uiso 1 1 calc R
N22 N -0.10885(12) -0.24033(19) 0.0086(2) 0.0416(7) Uani 1 1 d .
N28 N -0.13405(12) -0.0589(2) 0.0386(2) 0.0489(8) Uani 1 1 d .
N36 N -0.24691(13) -0.1764(3) 0.1890(3) 0.0600(9) Uani 1 1 d .
N39 N -0.22411(12) -0.3645(2) 0.1525(2) 0.0512(8) Uani 1 1 d .
C23 C -0.14288(13) -0.2289(2) 0.0531(2) 0.0341(7) Uani 1 1 d .
C24 C -0.16607(13) -0.3055(2) 0.0804(3) 0.0360(8) Uani 1 1 d .
C25 C -0.15445(14) -0.3982(2) 0.0598(3) 0.0433(9) Uani 1 1 d .
H25 H -0.1697 -0.4507 0.0764 0.052 Uiso 1 1 calc R
C26 C -0.12079(15) -0.4098(3) 0.0154(3) 0.0491(9) Uani 1 1 d .
H26 H -0.1124 -0.4703 0.0011 0.059 Uiso 1 1 calc R
C27 C -0.09893(15) -0.3293(3) -0.0082(3) 0.0478(9) Uani 1 1 d .
H27 H -0.0756 -0.3387 -0.0381 0.057 Uiso 1 1 calc R
C29 C -0.15594(13) -0.1304(2) 0.0692(3) 0.0369(8) Uani 1 1 d .
C30 C -0.19114(13) -0.1149(3) 0.1144(3) 0.0408(8) Uani 1 1 d .
C31 C -0.20472(16) -0.0208(3) 0.1242(3) 0.0582(11) Uani 1 1 d .
H31 H -0.2282 -0.0078 0.1530 0.070 Uiso 1 1 calc R
C32 C -0.18381(18) 0.0513(3) 0.0921(4) 0.0664(13) Uani 1 1 d .
H32 H -0.1929 0.1141 0.0979 0.080 Uiso 1 1 calc R
C33 C -0.14827(17) 0.0294(3) 0.0500(4) 0.0610(12) Uani 1 1 d .
H33 H -0.1337 0.0793 0.0287 0.073 Uiso 1 1 calc R
C34 C -0.20191(13) -0.2884(3) 0.1282(3) 0.0404(8) Uani 1 1 d .
C35 C -0.21376(13) -0.1951(3) 0.1455(3) 0.0422(8) Uani 1 1 d .
C37 C -0.26828(17) -0.2518(4) 0.2125(3) 0.0678(13) Uani 1 1 d .
H37 H -0.2912 -0.2425 0.2431 0.081 Uiso 1 1 calc R
C38 C -0.25769(16) -0.3441(4) 0.1933(3) 0.0631(12) Uani 1 1 d .
H38 H -0.2749 -0.3940 0.2097 0.076 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 93.23(13) 2 .
N9 Fe1 N4 89.51(10) . 2
N9 Fe1 N4 87.30(10) . .
N4 Fe1 N4 175.36(14) 2 .
N9 Fe1 N13 168.72(9) . 2
N4 Fe1 N13 87.20(10) . 2
N9 Fe1 N13 96.57(9) . .
N4 Fe1 N13 96.51(9) . .
N13 Fe1 N13 74.30(12) 2 .
C7 N3 N4 109.1(3) . .
C7 N3 B2 128.4(3) . .
N4 N3 B2 122.2(3) . .
C5 N4 N3 106.1(3) . .
C5 N4 Fe1 129.2(2) . .
N3 N4 Fe1 123.8(2) . .
C12 N8 N9 109.3(3) . .
C12 N8 B2 128.9(3) . .
N9 N8 B2 121.7(3) . .
C10 N9 N8 106.0(3) . .
C10 N9 Fe1 127.9(2) . .
N8 N9 Fe1 125.1(2) . .
C18 N13 C14 117.6(3) . .
C18 N13 Fe1 126.3(2) . .
C14 N13 Fe1 116.03(19) . .
C21 N20 C19 116.0(3) . .
N4 C5 C6 111.8(3) . .
N4 C5 H5 124.1 . .
C6 C5 H5 124.1 . .
C5 C6 C7 103.8(3) . .
C5 C6 H6 128.1 . .
C7 C6 H6 128.1 . .
N3 C7 C6 109.2(3) . .
N3 C7 H7 125.4 . .
C6 C7 H7 125.4 . .
N9 C10 C11 111.2(3) . .
N9 C10 H10 124.4 . .
C11 C10 H10 124.4 . .
C12 C11 C10 104.2(3) . .
C12 C11 H11 127.9 . .
C10 C11 H11 127.9 . .
N8 C12 C11 109.2(3) . .
N8 C12 H12 125.4 . .
C11 C12 H12 125.4 . .
N13 C14 C15 123.1(3) . .
N13 C14 C14 116.81(16) . 2
C15 C14 C14 120.13(18) . 2
C14 C15 C16 117.4(3) . .
C14 C15 C19 119.5(3) . .
C16 C15 C19 123.1(3) . .
C17 C16 C15 119.8(3) . .
C17 C16 H16 120.1 . .
C15 C16 H16 120.1 . .
C16 C17 C18 118.4(3) . .
C16 C17 H17 120.8 . .
C18 C17 H17 120.8 . .
N13 C18 C17 123.6(3) . .
N13 C18 H18 118.2 . .
C17 C18 H18 118.2 . .
N20 C19 C19 121.47(19) . 2
N20 C19 C15 118.2(3) . .
C19 C19 C15 120.32(17) 2 .
N20 C21 C21 122.5(2) . 2
N20 C21 H21 118.7 . .
C21 C21 H21 118.7 2 .
N3 B2 N8 110.0(3) . .
N3 B2 H2A 109.7 . .
N8 B2 H2A 109.7 . .
N3 B2 H2B 109.7 . .
N8 B2 H2B 109.7 . .
H2A B2 H2B 108.2 . .
C27 N22 C23 116.2(3) . .
C33 N28 C29 117.2(3) . .
C37 N36 C35 115.7(4) . .
C38 N39 C34 115.2(4) . .
N22 C23 C24 122.7(3) . .
N22 C23 C29 116.9(3) . .
C24 C23 C29 120.4(3) . .
C23 C24 C25 118.5(3) . .
C23 C24 C34 119.9(3) . .
C25 C24 C34 121.6(3) . .
C26 C25 C24 119.0(3) . .
C26 C25 H25 120.5 . .
C24 C25 H25 120.5 . .
C25 C26 C27 118.7(3) . .
C25 C26 H26 120.7 . .
C27 C26 H26 120.7 . .
N22 C27 C26 125.0(3) . .
N22 C27 H27 117.5 . .
C26 C27 H27 117.5 . .
N28 C29 C30 122.8(3) . .
N28 C29 C23 118.2(3) . .
C30 C29 C23 119.0(3) . .
C31 C30 C29 117.4(3) . .
C31 C30 C35 122.2(3) . .
C29 C30 C35 120.3(3) . .
C32 C31 C30 120.2(4) . .
C32 C31 H31 119.9 . .
C30 C31 H31 119.9 . .
C31 C32 C33 118.4(4) . .
C31 C32 H32 120.8 . .
C33 C32 H32 120.8 . .
N28 C33 C32 123.9(4) . .
N28 C33 H33 118.1 . .
C32 C33 H33 118.1 . .
N39 C34 C35 121.7(3) . .
N39 C34 C24 118.2(3) . .
C35 C34 C24 120.2(3) . .
N36 C35 C34 121.9(4) . .
N36 C35 C30 118.0(3) . .
C34 C35 C30 120.1(3) . .
N36 C37 C38 122.5(4) . .
N36 C37 H37 118.7 . .
C38 C37 H37 118.7 . .
N39 C38 C37 123.0(4) . .
N39 C38 H38 118.5 . .
C37 C38 H38 118.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N9 2.159(3) .
Fe1 N4 2.192(3) .
Fe1 N13 2.226(2) .
N3 C7 1.342(5) .
N3 N4 1.360(3) .
N3 B2 1.549(5) .
N4 C5 1.334(4) .
N8 C12 1.345(4) .
N8 N9 1.363(3) .
N8 B2 1.556(5) .
N9 C10 1.336(4) .
N13 C18 1.330(4) .
N13 C14 1.352(3) .
N20 C21 1.317(4) .
N20 C19 1.349(4) .
C5 C6 1.375(5) .
C5 H5 0.9300 .
C6 C7 1.381(5) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C10 C11 1.386(5) .
C10 H10 0.9300 .
C11 C12 1.372(5) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C14 C15 1.399(4) .
C14 C14 1.469(6) 2
C15 C16 1.401(4) .
C15 C19 1.457(4) .
C16 C17 1.372(5) .
C16 H16 0.9300 .
C17 C18 1.392(5) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 C19 1.402(6) 2
C21 C21 1.394(8) 2
C21 H21 0.9300 .
B2 H2A 0.9700 .
B2 H2B 0.9700 .
N22 C27 1.328(4) .
N22 C23 1.364(4) .
N28 C33 1.332(4) .
N28 C29 1.346(4) .
N36 C37 1.327(5) .
N36 C35 1.346(4) .
N39 C38 1.329(5) .
N39 C34 1.353(4) .
C23 C24 1.396(4) .
C23 C29 1.475(4) .
C24 C25 1.408(5) .
C24 C34 1.457(5) .
C25 C26 1.354(5) .
C25 H25 0.9300 .
C26 C27 1.392(5) .
C26 H26 0.9300 .
C27 H27 0.9300 .
C29 C30 1.407(4) .
C30 C31 1.396(5) .
C30 C35 1.455(5) .
C31 C32 1.350(6) .
C31 H31 0.9300 .
C32 C33 1.395(5) .
C32 H32 0.9300 .
C33 H33 0.9300 .
C34 C35 1.402(5) .
C37 C38 1.387(6) .
C37 H37 0.9300 .
C38 H38 0.9300 .
