#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:42:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179512 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/09/4340999.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_4340999
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                 119.380(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.1963(16)
_cell_length_b                   13.8773(6)
_cell_length_c                   14.9472(8)
_cell_measurement_reflns_used    3723
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      1.98
_cell_volume                     4734.9(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      140(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.841
_diffrn_measured_fraction_theta_max 0.841
_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  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0855
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13631
_diffrn_reflns_theta_full        29.78
_diffrn_reflns_theta_max         29.78
_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    0.384
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.819
_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    1.468
_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         -0.511
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0636
_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)+(0.0565P)²+3.9673P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1523
_reflns_number_gt                3982
_reflns_number_total             5701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501402q_si_003.cif
_cod_data_source_block           rk14a140
_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        4734.9(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4340999
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 0.26033(4) 0.2500 0.01699(16) Uani 1 2 d S
N3 N -0.12286(10) 0.30006(17) 0.07435(19) 0.0248(5) Uani 1 1 d .
N4 N -0.06872(10) 0.26443(16) 0.10143(18) 0.0228(5) Uani 1 1 d .
N8 N -0.09887(10) 0.38492(15) 0.23939(18) 0.0226(5) Uani 1 1 d .
N9 N -0.04003(10) 0.36519(16) 0.28987(18) 0.0237(5) Uani 1 1 d .
N13 N -0.03261(9) 0.14646(16) 0.29455(17) 0.0201(5) Uani 1 1 d .
N20 N -0.03439(10) -0.20186(17) 0.29868(19) 0.0269(6) Uani 1 1 d .
C5 C -0.06795(13) 0.2502(2) 0.0133(2) 0.0281(7) Uani 1 1 d .
H5 H -0.0354 0.2256 0.0091 0.034 Uiso 1 1 calc R
C6 C -0.12084(14) 0.2761(2) -0.0707(2) 0.0344(7) Uani 1 1 d .
H6 H -0.1316 0.2729 -0.1412 0.041 Uiso 1 1 calc R
C7 C -0.15427(13) 0.3074(2) -0.0287(2) 0.0331(7) Uani 1 1 d .
H7 H -0.1933 0.3306 -0.0664 0.040 Uiso 1 1 calc R
C10 C -0.01470(14) 0.43414(19) 0.3603(2) 0.0296(7) Uani 1 1 d .
H10 H 0.0262 0.4387 0.4063 0.035 Uiso 1 1 calc R
C11 C -0.05625(14) 0.4986(2) 0.3572(2) 0.0317(7) Uani 1 1 d .
H11 H -0.0498 0.5536 0.3993 0.038 Uiso 1 1 calc R
C12 C -0.10862(14) 0.4647(2) 0.2797(2) 0.0295(7) Uani 1 1 d .
H12 H -0.1459 0.4932 0.2580 0.035 Uiso 1 1 calc R
C14 C -0.01737(11) 0.05810(18) 0.2757(2) 0.0185(6) Uani 1 1 d .
C15 C -0.03364(11) -0.02835(19) 0.3026(2) 0.0205(6) Uani 1 1 d .
C16 C -0.06528(12) -0.0228(2) 0.3556(2) 0.0263(6) Uani 1 1 d .
H16 H -0.0768 -0.0798 0.3763 0.032 Uiso 1 1 calc R
C17 C -0.07936(12) 0.0661(2) 0.3771(2) 0.0277(7) Uani 1 1 d .
H17 H -0.1001 0.0714 0.4142 0.033 Uiso 1 1 calc R
C18 C -0.06314(12) 0.1485(2) 0.3443(2) 0.0249(6) Uani 1 1 d .
H18 H -0.0744 0.2094 0.3580 0.030 Uiso 1 1 calc R
C19 C -0.01665(11) -0.11890(18) 0.2751(2) 0.0222(6) Uani 1 1 d .
C21 C -0.01737(13) -0.2822(2) 0.2734(2) 0.0304(7) Uani 1 1 d .
H21 H -0.0293 -0.3422 0.2877 0.037 Uiso 1 1 calc R
B2 B -0.14402(13) 0.3198(2) 0.1525(3) 0.0236(7) Uani 1 1 d .
H2A H -0.1483 0.2582 0.1817 0.028 Uiso 1 1 calc R
H2B H -0.1827 0.3521 0.1179 0.028 Uiso 1 1 calc R
N22 N -0.10873(10) -0.24253(16) 0.00719(19) 0.0242(5) Uani 1 1 d .
N28 N -0.13516(10) -0.05804(16) 0.0341(2) 0.0271(6) Uani 1 1 d .
N36 N -0.24618(11) -0.1753(2) 0.1906(2) 0.0362(7) Uani 1 1 d .
N39 N -0.22301(10) -0.36605(19) 0.1557(2) 0.0321(6) Uani 1 1 d .
C23 C -0.14281(11) -0.22960(19) 0.0518(2) 0.0199(6) Uani 1 1 d .
C24 C -0.16567(11) -0.3073(2) 0.0807(2) 0.0216(6) Uani 1 1 d .
C25 C -0.15471(12) -0.4012(2) 0.0596(2) 0.0247(6) Uani 1 1 d .
H25 H -0.1701 -0.4552 0.0776 0.030 Uiso 1 1 calc R
C26 C -0.12172(12) -0.4138(2) 0.0129(2) 0.0285(7) Uani 1 1 d .
H26 H -0.1144 -0.4765 -0.0037 0.034 Uiso 1 1 calc R
C27 C -0.09891(12) -0.3324(2) -0.0099(2) 0.0263(6) Uani 1 1 d .
H27 H -0.0746 -0.3423 -0.0397 0.032 Uiso 1 1 calc R
C29 C -0.15626(11) -0.13075(19) 0.0674(2) 0.0214(6) Uani 1 1 d .
C30 C -0.19149(12) -0.1142(2) 0.1126(2) 0.0254(6) Uani 1 1 d .
C31 C -0.20600(13) -0.0186(2) 0.1206(3) 0.0339(7) Uani 1 1 d .
H31 H -0.2299 -0.0047 0.1505 0.041 Uiso 1 1 calc R
C32 C -0.18589(14) 0.0542(2) 0.0854(3) 0.0382(8) Uani 1 1 d .
H32 H -0.1961 0.1192 0.0890 0.046 Uiso 1 1 calc R
C33 C -0.14980(13) 0.0313(2) 0.0439(3) 0.0340(8) Uani 1 1 d .
H33 H -0.1349 0.0827 0.0214 0.041 Uiso 1 1 calc R
C34 C -0.20108(11) -0.2893(2) 0.1294(2) 0.0241(6) Uani 1 1 d .
C35 C -0.21323(12) -0.1947(2) 0.1457(2) 0.0264(6) Uani 1 1 d .
C37 C -0.26717(13) -0.2508(3) 0.2151(3) 0.0408(9) Uani 1 1 d .
H37 H -0.2908 -0.2405 0.2462 0.049 Uiso 1 1 calc R
C38 C -0.25627(13) -0.3455(3) 0.1974(2) 0.0398(9) Uani 1 1 d .
H38 H -0.2732 -0.3969 0.2158 0.048 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 89.33(12) . 2
N9 Fe1 N13 95.65(9) . .
N9 Fe1 N13 174.08(8) . 2
N13 Fe1 N13 79.56(12) . 2
N9 Fe1 N4 89.58(9) . .
N13 Fe1 N4 95.05(9) . .
N9 Fe1 N4 88.17(9) . 2
N13 Fe1 N4 87.38(9) . 2
N4 Fe1 N4 176.84(12) . 2
C7 N3 N4 109.3(2) . .
C7 N3 B2 127.4(2) . .
N4 N3 B2 123.2(2) . .
C5 N4 N3 106.0(2) . .
C5 N4 Fe1 128.9(2) . .
N3 N4 Fe1 124.15(18) . .
C12 N8 N9 109.1(2) . .
C12 N8 B2 128.5(2) . .
N9 N8 B2 122.4(2) . .
C10 N9 N8 106.3(2) . .
C10 N9 Fe1 127.8(2) . .
N8 N9 Fe1 125.48(17) . .
C18 N13 C14 116.8(2) . .
C18 N13 Fe1 128.50(19) . .
C14 N13 Fe1 114.52(16) . .
C21 N20 C19 115.9(3) . .
N4 C5 C6 111.2(3) . .
C7 C6 C5 104.3(3) . .
N3 C7 C6 109.2(3) . .
N9 C10 C11 110.9(3) . .
C12 C11 C10 104.4(3) . .
N8 C12 C11 109.2(3) . .
N13 C14 C15 123.6(2) . .
N13 C14 C14 115.67(14) . 2
C15 C14 C14 120.76(15) . 2
C14 C15 C16 117.6(2) . .
C14 C15 C19 118.8(2) . .
C16 C15 C19 123.6(2) . .
C17 C16 C15 118.9(3) . .
C16 C17 C18 119.6(3) . .
N13 C18 C17 123.4(3) . .
N20 C19 C19 121.55(16) . 2
N20 C19 C15 118.0(2) . .
C19 C19 C15 120.45(15) 2 .
N20 C21 C21 122.54(17) . 2
N3 B2 N8 109.2(2) . .
C27 N22 C23 117.0(2) . .
C33 N28 C29 117.5(2) . .
C37 N36 C35 115.7(3) . .
C38 N39 C34 115.9(3) . .
N22 C23 C24 122.1(2) . .
N22 C23 C29 117.9(2) . .
C24 C23 C29 120.0(2) . .
C23 C24 C25 118.7(2) . .
C23 C24 C34 119.7(2) . .
C25 C24 C34 121.5(2) . .
C26 C25 C24 119.0(3) . .
C25 C26 C27 118.5(3) . .
N22 C27 C26 124.6(3) . .
N28 C29 C30 122.5(2) . .
N28 C29 C23 117.7(2) . .
C30 C29 C23 119.8(2) . .
C31 C30 C29 117.8(3) . .
C31 C30 C35 122.2(3) . .
C29 C30 C35 120.0(3) . .
C32 C31 C30 119.9(3) . .
C31 C32 C33 118.5(3) . .
N28 C33 C32 123.8(3) . .
N39 C34 C35 121.4(3) . .
N39 C34 C24 118.4(3) . .
C35 C34 C24 120.2(3) . .
N36 C35 C34 121.8(3) . .
N36 C35 C30 118.0(3) . .
C34 C35 C30 120.2(2) . .
N36 C37 C38 123.0(3) . .
N39 C38 C37 122.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N9 2.046(2) .
Fe1 N13 2.056(2) .
Fe1 N4 2.062(2) .
N3 C7 1.348(4) .
N3 N4 1.363(3) .
N3 B2 1.544(4) .
N4 C5 1.342(4) .
N8 C12 1.343(3) .
N8 N9 1.371(3) .
N8 B2 1.547(4) .
N9 C10 1.333(4) .
N13 C18 1.333(3) .
N13 C14 1.361(3) .
N20 C21 1.323(4) .
N20 C19 1.351(3) .
C5 C6 1.385(4) .
C6 C7 1.374(4) .
C10 C11 1.392(4) .
C11 C12 1.374(4) .
C14 C15 1.396(4) .
C14 C14 1.452(5) 2
C15 C16 1.402(4) .
C15 C19 1.458(4) .
C16 C17 1.370(4) .
C17 C18 1.391(4) .
C19 C19 1.403(5) 2
C21 C21 1.394(6) 2
N22 C27 1.324(3) .
N22 C23 1.363(3) .
N28 C33 1.327(4) .
N28 C29 1.357(3) .
N36 C37 1.316(4) .
N36 C35 1.356(3) .
N39 C38 1.327(4) .
N39 C34 1.357(4) .
C23 C24 1.400(4) .
C23 C29 1.463(4) .
C24 C25 1.403(4) .
C24 C34 1.454(4) .
C25 C26 1.362(4) .
C26 C27 1.395(4) .
C29 C30 1.404(4) .
C30 C31 1.401(4) .
C30 C35 1.447(4) .
C31 C32 1.359(4) .
C32 C33 1.399(4) .
C34 C35 1.400(4) .
C37 C38 1.398(5) .
