#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:46:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179513 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/10/4341000.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_4341000
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                 119.179(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.2625(16)
_cell_length_b                   13.9405(7)
_cell_length_c                   14.9781(8)
_cell_measurement_reflns_used    3630
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      25.23
_cell_measurement_theta_min      2.01
_cell_volume                     4787.8(5)
_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      160(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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0854
_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            13873
_diffrn_reflns_theta_full        29.76
_diffrn_reflns_theta_max         29.76
_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    0.379
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.854
_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    1.452
_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         0.844
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0637
_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)+(0.0651P)²+1.9666P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1571
_reflns_number_gt                3966
_reflns_number_total             5768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501402q_si_003.cif
_cod_data_source_block           rk14a160
_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               4341000
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 0.26227(4) 0.2500 0.01940(16) Uani 1 2 d S
N3 N -0.12522(10) 0.30268(17) 0.07270(19) 0.0286(5) Uani 1 1 d .
N4 N -0.07111(10) 0.26766(16) 0.09803(19) 0.0264(5) Uani 1 1 d .
N8 N -0.10112(10) 0.38623(15) 0.23899(18) 0.0261(5) Uani 1 1 d .
N9 N -0.04276(10) 0.36773(15) 0.29052(18) 0.0263(5) Uani 1 1 d .
N13 N -0.03151(9) 0.14120(16) 0.29750(17) 0.0234(5) Uani 1 1 d .
N20 N -0.03359(10) -0.20516(17) 0.2994(2) 0.0315(6) Uani 1 1 d .
C5 C -0.07137(13) 0.2555(2) 0.0088(2) 0.0322(7) Uani 1 1 d .
H5 H -0.0392 0.2321 0.0029 0.039 Uiso 1 1 calc R
C6 C -0.12440(13) 0.2815(2) -0.0733(2) 0.0373(8) Uani 1 1 d .
H6 H -0.1357 0.2795 -0.1440 0.045 Uiso 1 1 calc R
C7 C -0.15715(14) 0.3109(2) -0.0291(2) 0.0404(8) Uani 1 1 d .
H7 H -0.1962 0.3334 -0.0652 0.048 Uiso 1 1 calc R
C10 C -0.01885(14) 0.4373(2) 0.3599(2) 0.0332(7) Uani 1 1 d .
H10 H 0.0217 0.4428 0.4064 0.040 Uiso 1 1 calc R
C11 C -0.06080(15) 0.5004(2) 0.3555(2) 0.0380(8) Uani 1 1 d .
H11 H -0.0552 0.5553 0.3969 0.046 Uiso 1 1 calc R
C12 C -0.11223(15) 0.4656(2) 0.2778(2) 0.0360(7) Uani 1 1 d .
H12 H -0.1497 0.4931 0.2550 0.043 Uiso 1 1 calc R
C14 C -0.01696(11) 0.05411(18) 0.2768(2) 0.0214(6) Uani 1 1 d .
C15 C -0.03277(11) -0.03215(19) 0.3038(2) 0.0228(6) Uani 1 1 d .
C16 C -0.06372(11) -0.0275(2) 0.3580(2) 0.0287(7) Uani 1 1 d .
H16 H -0.0751 -0.0846 0.3781 0.034 Uiso 1 1 calc R
C17 C -0.07741(12) 0.0606(2) 0.3816(2) 0.0313(7) Uani 1 1 d .
H17 H -0.0978 0.0653 0.4193 0.038 Uiso 1 1 calc R
C18 C -0.06096(11) 0.1430(2) 0.3494(2) 0.0274(6) Uani 1 1 d .
H18 H -0.0712 0.2036 0.3651 0.033 Uiso 1 1 calc R
C19 C -0.01631(11) -0.12243(18) 0.2756(2) 0.0252(6) Uani 1 1 d .
C21 C -0.01719(13) -0.2848(2) 0.2741(2) 0.0352(7) Uani 1 1 d .
H21 H -0.0289 -0.3445 0.2889 0.042 Uiso 1 1 calc R
B2 B -0.14499(14) 0.3194(2) 0.1536(3) 0.0286(7) Uani 1 1 d .
H2A H -0.1843 0.3488 0.1206 0.034 Uiso 1 1 calc R
H2B H -0.1472 0.2572 0.1834 0.034 Uiso 1 1 calc R
N22 N -0.10855(10) -0.24155(16) 0.0084(2) 0.0269(5) Uani 1 1 d .
N28 N -0.13431(10) -0.05852(16) 0.0369(2) 0.0312(6) Uani 1 1 d .
N36 N -0.24699(10) -0.1762(2) 0.1895(2) 0.0392(7) Uani 1 1 d .
N39 N -0.22397(10) -0.36587(18) 0.15363(19) 0.0334(6) Uani 1 1 d .
C23 C -0.14240(11) -0.22969(19) 0.0526(2) 0.0230(6) Uani 1 1 d .
C24 C -0.16596(11) -0.30690(19) 0.0805(2) 0.0242(6) Uani 1 1 d .
C25 C -0.15515(12) -0.4003(2) 0.0591(2) 0.0284(6) Uani 1 1 d .
H25 H -0.1710 -0.4542 0.0759 0.034 Uiso 1 1 calc R
C26 C -0.12148(12) -0.4125(2) 0.0138(2) 0.0315(7) Uani 1 1 d .
H26 H -0.1135 -0.4750 -0.0016 0.038 Uiso 1 1 calc R
C27 C -0.09892(12) -0.3315(2) -0.0095(2) 0.0308(7) Uani 1 1 d .
H27 H -0.0751 -0.3412 -0.0402 0.037 Uiso 1 1 calc R
C29 C -0.15578(11) -0.13062(19) 0.0689(2) 0.0232(6) Uani 1 1 d .
C30 C -0.19122(11) -0.1147(2) 0.1137(2) 0.0270(6) Uani 1 1 d .
C31 C -0.20534(13) -0.0196(2) 0.1229(2) 0.0361(7) Uani 1 1 d .
H31 H -0.2293 -0.0060 0.1525 0.043 Uiso 1 1 calc R
C32 C -0.18452(14) 0.0532(2) 0.0891(3) 0.0429(9) Uani 1 1 d .
H32 H -0.1942 0.1180 0.0937 0.051 Uiso 1 1 calc R
C33 C -0.14852(13) 0.0306(2) 0.0476(3) 0.0388(8) Uani 1 1 d .
H33 H -0.1334 0.0818 0.0257 0.047 Uiso 1 1 calc R
C34 C -0.20197(11) -0.2893(2) 0.1283(2) 0.0258(6) Uani 1 1 d .
C35 C -0.21359(11) -0.1949(2) 0.1456(2) 0.0283(6) Uani 1 1 d .
C37 C -0.26853(14) -0.2515(3) 0.2131(3) 0.0429(9) Uani 1 1 d .
H37 H -0.2923 -0.2414 0.2438 0.052 Uiso 1 1 calc R
C38 C -0.25766(12) -0.3455(3) 0.1945(2) 0.0418(8) Uani 1 1 d .
H38 H -0.2750 -0.3968 0.2118 0.050 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 91.70(12) 2 .
N9 Fe1 N4 88.87(9) . 2
N9 Fe1 N4 88.31(9) . .
N4 Fe1 N4 175.95(12) 2 .
N9 Fe1 N13 96.16(8) . .
N4 Fe1 N13 95.92(8) . .
N9 Fe1 N13 170.90(8) . 2
N4 Fe1 N13 87.27(8) . 2
N13 Fe1 N13 76.41(11) . 2
C7 N3 N4 109.6(2) . .
C7 N3 B2 127.9(2) . .
N4 N3 B2 122.3(2) . .
C5 N4 N3 105.5(2) . .
C5 N4 Fe1 129.5(2) . .
N3 N4 Fe1 124.04(18) . .
C12 N8 N9 109.4(2) . .
C12 N8 B2 128.4(2) . .
N9 N8 B2 122.2(2) . .
C10 N9 N8 106.0(2) . .
C10 N9 Fe1 128.0(2) . .
N8 N9 Fe1 125.31(17) . .
C18 N13 C14 117.3(2) . .
C18 N13 Fe1 127.09(18) . .
C14 N13 Fe1 115.56(16) . .
C21 N20 C19 116.6(3) . .
N4 C5 C6 111.5(3) . .
N4 C5 H5 124.3 . .
C6 C5 H5 124.3 . .
C7 C6 C5 104.1(3) . .
C7 C6 H6 127.9 . .
C5 C6 H6 127.9 . .
N3 C7 C6 109.3(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 104.3(3) . .
C12 C11 H11 127.9 . .
C10 C11 H11 127.9 . .
N8 C12 C11 109.0(3) . .
N8 C12 H12 125.5 . .
C11 C12 H12 125.5 . .
N13 C14 C15 123.3(2) . .
N13 C14 C14 116.22(14) . 2
C15 C14 C14 120.47(15) . 2
C14 C15 C16 117.8(2) . .
C14 C15 C19 119.1(2) . .
C16 C15 C19 123.0(2) . .
C17 C16 C15 119.3(3) . .
C17 C16 H16 120.4 . .
C15 C16 H16 120.4 . .
C16 C17 C18 118.9(3) . .
C16 C17 H17 120.5 . .
C18 C17 H17 120.5 . .
N13 C18 C17 123.4(3) . .
N13 C18 H18 118.3 . .
C17 C18 H18 118.3 . .
N20 C19 C19 121.25(16) . 2
N20 C19 C15 118.4(2) . .
C19 C19 C15 120.36(14) 2 .
N20 C21 C21 122.15(17) . 2
N20 C21 H21 118.9 . .
C21 C21 H21 118.9 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 116.6(2) . .
C33 N28 C29 117.6(3) . .
C37 N36 C35 116.1(3) . .
C38 N39 C34 115.5(3) . .
N22 C23 C24 122.9(2) . .
N22 C23 C29 117.5(2) . .
C24 C23 C29 119.6(2) . .
C23 C24 C25 118.5(2) . .
C23 C24 C34 120.2(2) . .
C25 C24 C34 121.3(2) . .
C26 C25 C24 118.8(3) . .
C26 C25 H25 120.6 . .
C24 C25 H25 120.6 . .
C25 C26 C27 118.8(3) . .
C25 C26 H26 120.6 . .
C27 C26 H26 120.6 . .
N22 C27 C26 124.4(3) . .
N22 C27 H27 117.8 . .
C26 C27 H27 117.8 . .
N28 C29 C30 122.8(2) . .
N28 C29 C23 117.7(2) . .
C30 C29 C23 119.6(2) . .
C31 C30 C29 117.6(3) . .
C31 C30 C35 122.0(3) . .
C29 C30 C35 120.4(2) . .
C32 C31 C30 119.7(3) . .
C32 C31 H31 120.1 . .
C30 C31 H31 120.1 . .
C31 C32 C33 118.6(3) . .
C31 C32 H32 120.7 . .
C33 C32 H32 120.7 . .
N28 C33 C32 123.7(3) . .
N28 C33 H33 118.2 . .
C32 C33 H33 118.2 . .
N39 C34 C35 121.8(3) . .
N39 C34 C24 118.2(3) . .
C35 C34 C24 120.0(3) . .
N36 C35 C34 121.4(3) . .
N36 C35 C30 118.3(3) . .
C34 C35 C30 120.3(2) . .
N36 C37 C38 122.4(3) . .
N36 C37 H37 118.8 . .
C38 C37 H37 118.8 . .
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 2.111(2) .
Fe1 N4 2.128(2) .
Fe1 N13 2.148(2) .
N3 C7 1.339(4) .
N3 N4 1.370(3) .
N3 B2 1.550(4) .
N4 C5 1.344(4) .
N8 C12 1.346(4) .
N8 N9 1.363(3) .
N8 B2 1.548(4) .
N9 C10 1.334(4) .
N13 C18 1.338(3) .
N13 C14 1.353(3) .
N20 C21 1.312(4) .
N20 C19 1.349(3) .
C5 C6 1.383(4) .
C5 H5 0.9500 .
C6 C7 1.379(4) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C10 C11 1.386(4) .
C10 H10 0.9500 .
C11 C12 1.372(4) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C14 C15 1.395(4) .
C14 C14 1.461(5) 2
C15 C16 1.402(4) .
C15 C19 1.459(4) .
C16 C17 1.374(4) .
C16 H16 0.9500 .
C17 C18 1.393(4) .
C17 H17 0.9500 .
C18 H18 0.9500 .
C19 C19 1.401(5) 2
C21 C21 1.405(6) 2
C21 H21 0.9500 .
B2 H2A 0.9900 .
B2 H2B 0.9900 .
N22 C27 1.332(3) .
N22 C23 1.352(3) .
N28 C33 1.329(4) .
N28 C29 1.349(3) .
N36 C37 1.320(4) .
N36 C35 1.354(3) .
N39 C38 1.329(4) .
N39 C34 1.353(4) .
C23 C24 1.403(4) .
C23 C29 1.475(4) .
C24 C25 1.403(4) .
C24 C34 1.459(4) .
C25 C26 1.362(4) .
C25 H25 0.9500 .
C26 C27 1.397(4) .
C26 H26 0.9500 .
C27 H27 0.9500 .
C29 C30 1.406(4) .
C30 C31 1.402(4) .
C30 C35 1.447(4) .
C31 C32 1.362(4) .
C31 H31 0.9500 .
C32 C33 1.398(4) .
C32 H32 0.9500 .
C33 H33 0.9500 .
C34 C35 1.403(4) .
C37 C38 1.398(5) .
C37 H37 0.9500 .
C38 H38 0.9500 .
