#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:46:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179513 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/10/4341006.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_4341006
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                 118.746(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.373(3)
_cell_length_b                   14.0634(10)
_cell_length_c                   15.0757(15)
_cell_measurement_reflns_used    2373
_cell_measurement_temperature    280(2)
_cell_measurement_theta_max      24.60
_cell_measurement_theta_min      1.98
_cell_volume                     4902.4(9)
_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      280(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  0.0780
_diffrn_reflns_av_sigmaI/netI    0.1270
_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            14131
_diffrn_reflns_theta_full        29.75
_diffrn_reflns_theta_max         29.75
_diffrn_reflns_theta_min         1.69
_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  0.885
_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    1.418
_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         0.606
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1546
_refine_ls_R_factor_gt           0.0718
_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)+(0.0590P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1788
_reflns_number_gt                3037
_reflns_number_total             5897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501402q_si_003.cif
_cod_data_source_block           rk14a280
_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        4902.4(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4341006
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 0.26263(4) 0.2500 0.0334(2) Uani 1 2 d S
N3 N -0.12594(12) 0.3037(2) 0.0733(3) 0.0456(8) Uani 1 1 d .
N4 N -0.07297(11) 0.26907(19) 0.0958(2) 0.0394(7) Uani 1 1 d .
N8 N -0.10232(12) 0.38610(18) 0.2387(2) 0.0424(8) Uani 1 1 d .
N9 N -0.04450(11) 0.36801(18) 0.2911(2) 0.0388(7) Uani 1 1 d .
N13 N -0.03055(11) 0.13655(18) 0.3000(2) 0.0363(7) Uani 1 1 d .
N20 N -0.03289(13) -0.2064(2) 0.3002(3) 0.0529(9) Uani 1 1 d .
C5 C -0.07329(16) 0.2578(2) 0.0078(3) 0.0462(10) Uani 1 1 d .
H5 H -0.0421 0.2348 0.0015 0.055 Uiso 1 1 calc R
C6 C -0.12535(17) 0.2844(3) -0.0726(3) 0.0566(11) Uani 1 1 d .
H6 H -0.1363 0.2833 -0.1411 0.068 Uiso 1 1 calc R
C7 C -0.15729(17) 0.3130(3) -0.0274(4) 0.0640(12) Uani 1 1 d .
H7 H -0.1951 0.3355 -0.0616 0.077 Uiso 1 1 calc R
C10 C -0.02161(16) 0.4376(2) 0.3587(3) 0.0482(10) Uani 1 1 d .
H10 H 0.0176 0.4435 0.4041 0.058 Uiso 1 1 calc R
C11 C -0.06339(19) 0.4997(2) 0.3529(3) 0.0566(11) Uani 1 1 d .
H11 H -0.0584 0.5532 0.3925 0.068 Uiso 1 1 calc R
C12 C -0.11370(19) 0.4652(3) 0.2763(3) 0.0543(11) Uani 1 1 d .
H12 H -0.1501 0.4921 0.2535 0.065 Uiso 1 1 calc R
C14 C -0.01646(12) 0.0508(2) 0.2776(3) 0.0319(8) Uani 1 1 d .
C15 C -0.03196(13) -0.0351(2) 0.3048(3) 0.0367(9) Uani 1 1 d .
C16 C -0.06237(14) -0.0307(3) 0.3593(3) 0.0452(10) Uani 1 1 d .
H16 H -0.0734 -0.0863 0.3787 0.054 Uiso 1 1 calc R
C17 C -0.07582(15) 0.0562(3) 0.3841(3) 0.0499(10) Uani 1 1 d .
H17 H -0.0953 0.0606 0.4215 0.060 Uiso 1 1 calc R
C18 C -0.05941(14) 0.1378(2) 0.3517(3) 0.0439(9) Uani 1 1 d .
H18 H -0.0693 0.1965 0.3673 0.053 Uiso 1 1 calc R
C19 C -0.01615(13) -0.1248(2) 0.2758(3) 0.0404(9) Uani 1 1 d .
C21 C -0.01682(17) -0.2853(2) 0.2746(4) 0.0611(13) Uani 1 1 d .
H21 H -0.0281 -0.3432 0.2894 0.073 Uiso 1 1 calc R
B2 B -0.14469(18) 0.3180(3) 0.1547(4) 0.0532(13) Uani 1 1 d .
H2A H -0.1453 0.2571 0.1844 0.064 Uiso 1 1 calc R
H2B H -0.1834 0.3443 0.1239 0.064 Uiso 1 1 calc R
N22 N -0.10897(13) -0.2398(2) 0.0091(3) 0.0461(8) Uani 1 1 d .
N28 N -0.13400(12) -0.0589(2) 0.0385(3) 0.0517(9) Uani 1 1 d .
N36 N -0.24706(14) -0.1762(3) 0.1895(3) 0.0655(10) Uani 1 1 d .
N39 N -0.22397(13) -0.3642(2) 0.1522(3) 0.0572(9) Uani 1 1 d .
C23 C -0.14300(13) -0.2284(2) 0.0527(3) 0.0377(9) Uani 1 1 d .
C24 C -0.16569(13) -0.3051(2) 0.0809(3) 0.0401(9) Uani 1 1 d .
C25 C -0.15452(15) -0.3974(3) 0.0599(3) 0.0468(10) Uani 1 1 d .
H25 H -0.1701 -0.4497 0.0759 0.056 Uiso 1 1 calc R
C26 C -0.12077(17) -0.4092(3) 0.0160(3) 0.0573(11) Uani 1 1 d .
H26 H -0.1123 -0.4698 0.0021 0.069 Uiso 1 1 calc R
C27 C -0.09895(15) -0.3292(3) -0.0077(3) 0.0540(11) Uani 1 1 d .
H27 H -0.0756 -0.3386 -0.0374 0.065 Uiso 1 1 calc R
C29 C -0.15596(13) -0.1304(2) 0.0693(3) 0.0392(9) Uani 1 1 d .
C30 C -0.19102(14) -0.1147(3) 0.1141(3) 0.0444(10) Uani 1 1 d .
C31 C -0.20476(17) -0.0212(3) 0.1243(4) 0.0636(13) Uani 1 1 d .
H31 H -0.2283 -0.0083 0.1529 0.076 Uiso 1 1 calc R
C32 C -0.18354(19) 0.0507(3) 0.0922(4) 0.0756(15) Uani 1 1 d .
H32 H -0.1925 0.1135 0.0983 0.091 Uiso 1 1 calc R
C33 C -0.14800(18) 0.0295(3) 0.0496(4) 0.0660(13) Uani 1 1 d .
H33 H -0.1335 0.0795 0.0281 0.079 Uiso 1 1 calc R
C34 C -0.20187(13) -0.2879(3) 0.1285(3) 0.0430(9) Uani 1 1 d .
C35 C -0.21371(14) -0.1946(3) 0.1459(3) 0.0467(10) Uani 1 1 d .
C37 C -0.26802(18) -0.2522(4) 0.2124(4) 0.0747(15) Uani 1 1 d .
H37 H -0.2913 -0.2433 0.2424 0.090 Uiso 1 1 calc R
C38 C -0.25704(17) -0.3446(4) 0.1938(4) 0.0722(14) Uani 1 1 d .
H38 H -0.2736 -0.3947 0.2112 0.087 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 93.25(14) . 2
N9 Fe1 N4 87.40(11) . .
N9 Fe1 N4 89.34(11) . 2
N4 Fe1 N4 175.27(14) . 2
N9 Fe1 N13 96.59(10) . .
N4 Fe1 N13 96.65(10) . .
N9 Fe1 N13 168.70(9) . 2
N4 Fe1 N13 87.14(10) . 2
N13 Fe1 N13 74.24(14) . 2
C7 N3 N4 108.5(3) . .
C7 N3 B2 129.0(3) . .
N4 N3 B2 122.2(3) . .
C5 N4 N3 106.3(3) . .
C5 N4 Fe1 129.2(2) . .
N3 N4 Fe1 123.5(2) . .
C12 N8 N9 108.9(3) . .
C12 N8 B2 129.4(3) . .
N9 N8 B2 121.6(3) . .
C10 N9 N8 106.0(3) . .
C10 N9 Fe1 128.0(2) . .
N8 N9 Fe1 125.0(2) . .
C18 N13 C14 117.6(3) . .
C18 N13 Fe1 126.4(2) . .
C14 N13 Fe1 116.0(2) . .
C21 N20 C19 116.5(4) . .
N4 C5 C6 111.7(3) . .
N4 C5 H5 124.1 . .
C6 C5 H5 124.1 . .
C7 C6 C5 103.5(4) . .
C7 C6 H6 128.3 . .
C5 C6 H6 128.3 . .
N3 C7 C6 109.9(3) . .
N3 C7 H7 125.0 . .
C6 C7 H7 125.0 . .
N9 C10 C11 111.4(3) . .
N9 C10 H10 124.3 . .
C11 C10 H10 124.3 . .
C12 C11 C10 104.6(3) . .
C12 C11 H11 127.7 . .
C10 C11 H11 127.7 . .
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 116.86(18) . 2
C15 C14 C14 120.26(19) . 2
C14 C15 C16 117.7(3) . .
C14 C15 C19 119.5(3) . .
C16 C15 C19 122.8(3) . .
C17 C16 C15 119.7(3) . .
C17 C16 H16 120.2 . .
C15 C16 H16 120.2 . .
C16 C17 C18 118.2(3) . .
C16 C17 H17 120.9 . .
C18 C17 H17 120.9 . .
N13 C18 C17 123.9(3) . .
N13 C18 H18 118.1 . .
C17 C18 H18 118.1 . .
N20 C19 C19 121.3(2) . 2
N20 C19 C15 118.5(3) . .
C19 C19 C15 120.20(19) 2 .
N20 C21 C21 122.2(2) . 2
N20 C21 H21 118.9 . .
C21 C21 H21 118.9 2 .
N3 B2 N8 110.4(3) . .
N3 B2 H2A 109.6 . .
N8 B2 H2A 109.6 . .
N3 B2 H2B 109.6 . .
N8 B2 H2B 109.6 . .
H2A B2 H2B 108.1 . .
C27 N22 C23 116.2(3) . .
C33 N28 C29 117.5(3) . .
C37 N36 C35 115.0(4) . .
C38 N39 C34 115.2(4) . .
N22 C23 C24 122.5(3) . .
N22 C23 C29 117.2(3) . .
C24 C23 C29 120.3(3) . .
C23 C24 C25 118.7(3) . .
C23 C24 C34 119.8(3) . .
C25 C24 C34 121.5(3) . .
C26 C25 C24 119.0(4) . .
C26 C25 H25 120.5 . .
C24 C25 H25 120.5 . .
C25 C26 C27 118.6(4) . .
C25 C26 H26 120.7 . .
C27 C26 H26 120.7 . .
N22 C27 C26 124.9(4) . .
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 117.9(4) . .
C31 C30 C35 121.5(4) . .
C29 C30 C35 120.5(3) . .
C32 C31 C30 119.5(4) . .
C32 C31 H31 120.2 . .
C30 C31 H31 120.2 . .
C31 C32 C33 119.2(4) . .
C31 C32 H32 120.4 . .
C33 C32 H32 120.4 . .
N28 C33 C32 123.0(4) . .
N28 C33 H33 118.5 . .
C32 C33 H33 118.5 . .
N39 C34 C35 122.1(3) . .
N39 C34 C24 117.7(3) . .
C35 C34 C24 120.2(3) . .
N36 C35 C34 121.7(4) . .
N36 C35 C30 118.5(4) . .
C34 C35 C30 119.7(3) . .
N36 C37 C38 123.3(4) . .
N36 C37 H37 118.3 . .
C38 C37 H37 118.3 . .
N39 C38 C37 122.6(4) . .
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 2.158(3) .
Fe1 N4 2.194(3) .
Fe1 N13 2.224(3) .
N3 C7 1.341(5) .
N3 N4 1.359(4) .
N3 B2 1.542(6) .
N4 C5 1.332(5) .
N8 C12 1.346(4) .
N8 N9 1.362(4) .
N8 B2 1.552(5) .
N9 C10 1.330(4) .
N13 C18 1.326(4) .
N13 C14 1.352(4) .
N20 C21 1.311(5) .
N20 C19 1.344(4) .
C5 C6 1.376(5) .
C5 H5 0.9300 .
C6 C7 1.374(6) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C10 C11 1.376(5) .
C10 H10 0.9300 .
C11 C12 1.362(5) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C14 C15 1.398(4) .
C14 C14 1.463(6) 2
C15 C16 1.399(5) .
C15 C19 1.461(4) .
C16 C17 1.373(5) .
C16 H16 0.9300 .
C17 C18 1.395(5) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 C19 1.402(7) 2
C21 C21 1.403(9) 2
C21 H21 0.9300 .
B2 H2A 0.9700 .
B2 H2B 0.9700 .
N22 C27 1.335(4) .
N22 C23 1.353(4) .
N28 C33 1.330(5) .
N28 C29 1.349(4) .
N36 C37 1.323(6) .
N36 C35 1.353(5) .
N39 C38 1.325(5) .
N39 C34 1.350(4) .
C23 C24 1.395(5) .
C23 C29 1.470(5) .
C24 C25 1.400(5) .
C24 C34 1.464(5) .
C25 C26 1.350(5) .
C25 H25 0.9300 .
C26 C27 1.387(5) .
C26 H26 0.9300 .
C27 H27 0.9300 .
C29 C30 1.401(5) .
C30 C31 1.392(5) .
C30 C35 1.458(5) .
C31 C32 1.353(6) .
C31 H31 0.9300 .
C32 C33 1.400(6) .
C32 H32 0.9300 .
C33 H33 0.9300 .
C34 C35 1.402(5) .
C37 C38 1.390(6) .
C37 H37 0.9300 .
C38 H38 0.9300 .
