#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:46:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179513 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/10/4341007.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_4341007
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                 118.693(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.381(3)
_cell_length_b                   14.0694(10)
_cell_length_c                   15.0785(15)
_cell_measurement_reflns_used    2278
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      24.58
_cell_measurement_theta_min      1.97
_cell_volume                     4909.4(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      290(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.836
_diffrn_measured_fraction_theta_max 0.836
_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  0.0799
_diffrn_reflns_av_sigmaI/netI    0.1133
_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            14119
_diffrn_reflns_theta_full        29.85
_diffrn_reflns_theta_max         29.85
_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    0.370
_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    1.416
_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         0.618
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.065
_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         5910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1620
_refine_ls_R_factor_gt           0.0736
_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)+(0.0596P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1857
_reflns_number_gt                3026
_reflns_number_total             5910
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501402q_si_003.cif
_cod_data_source_block           rk14a290
_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        4909.4(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4341007
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 0.26238(5) 0.2500 0.0353(2) Uani 1 2 d S
N3 N -0.12567(12) 0.3032(2) 0.0731(3) 0.0477(8) Uani 1 1 d .
N4 N -0.07273(12) 0.2686(2) 0.0967(3) 0.0419(8) Uani 1 1 d .
N8 N -0.10226(12) 0.3858(2) 0.2386(2) 0.0439(8) Uani 1 1 d .
N9 N -0.04452(12) 0.36794(19) 0.2910(2) 0.0402(7) Uani 1 1 d .
N13 N -0.03074(11) 0.13657(19) 0.3001(2) 0.0386(7) Uani 1 1 d .
N20 N -0.03305(13) -0.2062(2) 0.3002(3) 0.0552(9) Uani 1 1 d .
C5 C -0.07313(17) 0.2578(3) 0.0086(3) 0.0490(10) Uani 1 1 d .
H5 H -0.0419 0.2351 0.0022 0.059 Uiso 1 1 calc R
C6 C -0.12508(18) 0.2842(3) -0.0717(4) 0.0609(12) Uani 1 1 d .
H6 H -0.1361 0.2830 -0.1402 0.073 Uiso 1 1 calc R
C7 C -0.15698(17) 0.3128(3) -0.0262(4) 0.0638(13) Uani 1 1 d .
H7 H -0.1947 0.3355 -0.0600 0.077 Uiso 1 1 calc R
C10 C -0.02142(17) 0.4371(3) 0.3585(3) 0.0521(11) Uani 1 1 d .
H10 H 0.0178 0.4428 0.4036 0.063 Uiso 1 1 calc R
C11 C -0.0633(2) 0.4999(3) 0.3531(4) 0.0582(12) Uani 1 1 d .
H11 H -0.0583 0.5535 0.3925 0.070 Uiso 1 1 calc R
C12 C -0.1132(2) 0.4650(3) 0.2772(4) 0.0592(12) Uani 1 1 d .
H12 H -0.1496 0.4916 0.2549 0.071 Uiso 1 1 calc R
C14 C -0.01635(13) 0.0509(2) 0.2779(3) 0.0343(8) Uani 1 1 d .
C15 C -0.03198(13) -0.0348(2) 0.3051(3) 0.0377(9) Uani 1 1 d .
C16 C -0.06245(14) -0.0303(3) 0.3592(3) 0.0472(10) Uani 1 1 d .
H16 H -0.0736 -0.0860 0.3784 0.057 Uiso 1 1 calc R
C17 C -0.07591(15) 0.0562(3) 0.3839(3) 0.0511(11) Uani 1 1 d .
H17 H -0.0953 0.0605 0.4214 0.061 Uiso 1 1 calc R
C18 C -0.05973(15) 0.1373(3) 0.3511(3) 0.0449(10) Uani 1 1 d .
H18 H -0.0700 0.1960 0.3662 0.054 Uiso 1 1 calc R
C19 C -0.01608(13) -0.1245(2) 0.2758(3) 0.0400(9) Uani 1 1 d .
C21 C -0.01673(17) -0.2852(3) 0.2745(4) 0.0649(14) Uani 1 1 d .
H21 H -0.0279 -0.3431 0.2894 0.078 Uiso 1 1 calc R
B2 B -0.14508(19) 0.3181(3) 0.1541(4) 0.0535(13) Uani 1 1 d .
H2A H -0.1463 0.2574 0.1834 0.064 Uiso 1 1 calc R
H2B H -0.1836 0.3452 0.1228 0.064 Uiso 1 1 calc R
N22 N -0.10881(13) -0.2399(2) 0.0090(3) 0.0495(9) Uani 1 1 d .
N28 N -0.13453(13) -0.0590(2) 0.0374(3) 0.0586(10) Uani 1 1 d .
N36 N -0.24684(14) -0.1767(3) 0.1898(3) 0.0691(11) Uani 1 1 d .
N39 N -0.22384(13) -0.3635(3) 0.1525(3) 0.0606(10) Uani 1 1 d .
C23 C -0.14292(14) -0.2285(2) 0.0527(3) 0.0403(9) Uani 1 1 d .
C24 C -0.16577(14) -0.3047(3) 0.0810(3) 0.0418(9) Uani 1 1 d .
C25 C -0.15453(16) -0.3970(3) 0.0602(3) 0.0507(10) Uani 1 1 d .
H25 H -0.1699 -0.4494 0.0766 0.061 Uiso 1 1 calc R
C26 C -0.12106(17) -0.4087(3) 0.0160(4) 0.0582(12) Uani 1 1 d .
H26 H -0.1128 -0.4692 0.0018 0.070 Uiso 1 1 calc R
C27 C -0.09898(17) -0.3286(3) -0.0081(4) 0.0593(12) Uani 1 1 d .
H27 H -0.0758 -0.3381 -0.0381 0.071 Uiso 1 1 calc R
C29 C -0.15593(14) -0.1304(3) 0.0694(3) 0.0425(9) Uani 1 1 d .
C30 C -0.19097(15) -0.1146(3) 0.1143(3) 0.0475(10) Uani 1 1 d .
C31 C -0.20453(17) -0.0209(3) 0.1244(4) 0.0661(13) Uani 1 1 d .
H31 H -0.2278 -0.0077 0.1535 0.079 Uiso 1 1 calc R
C32 C -0.1834(2) 0.0510(3) 0.0914(4) 0.0794(16) Uani 1 1 d .
H32 H -0.1923 0.1139 0.0969 0.095 Uiso 1 1 calc R
C33 C -0.14816(19) 0.0287(3) 0.0494(4) 0.0710(14) Uani 1 1 d .
H33 H -0.1333 0.0785 0.0284 0.085 Uiso 1 1 calc R
C34 C -0.20175(14) -0.2872(3) 0.1286(3) 0.0462(10) Uani 1 1 d .
C35 C -0.21343(15) -0.1941(3) 0.1453(3) 0.0499(10) Uani 1 1 d .
C37 C -0.26784(19) -0.2510(5) 0.2130(4) 0.0785(16) Uani 1 1 d .
H37 H -0.2909 -0.2416 0.2434 0.094 Uiso 1 1 calc R
C38 C -0.25707(18) -0.3440(4) 0.1940(4) 0.0756(15) Uani 1 1 d .
H38 H -0.2738 -0.3940 0.2110 0.091 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 93.10(15) . 2
N9 Fe1 N4 87.30(11) . .
N9 Fe1 N4 89.52(11) . 2
N4 Fe1 N4 175.38(15) . 2
N9 Fe1 N13 96.49(10) . .
N4 Fe1 N13 96.50(11) . .
N9 Fe1 N13 168.89(10) . 2
N4 Fe1 N13 87.18(11) . 2
N13 Fe1 N13 74.58(14) . 2
C7 N3 N4 109.8(3) . .
C7 N3 B2 127.9(3) . .
N4 N3 B2 122.0(3) . .
C5 N4 N3 105.4(3) . .
C5 N4 Fe1 129.3(2) . .
N3 N4 Fe1 124.3(3) . .
C12 N8 N9 108.3(3) . .
C12 N8 B2 129.5(3) . .
N9 N8 B2 122.1(3) . .
C10 N9 N8 106.5(3) . .
C10 N9 Fe1 127.7(2) . .
N8 N9 Fe1 124.9(2) . .
C18 N13 C14 117.5(3) . .
C18 N13 Fe1 126.8(2) . .
C14 N13 Fe1 115.7(2) . .
C21 N20 C19 116.1(4) . .
N4 C5 C6 112.0(4) . .
N4 C5 H5 124.0 . .
C6 C5 H5 124.0 . .
C5 C6 C7 103.3(4) . .
C5 C6 H6 128.3 . .
C7 C6 H6 128.3 . .
N3 C7 C6 109.5(4) . .
N3 C7 H7 125.2 . .
C6 C7 H7 125.2 . .
N9 C10 C11 111.3(4) . .
N9 C10 H10 124.4 . .
C11 C10 H10 124.4 . .
C12 C11 C10 104.0(4) . .
C12 C11 H11 128.0 . .
C10 C11 H11 128.0 . .
N8 C12 C11 109.9(3) . .
N8 C12 H12 125.0 . .
C11 C12 H12 125.0 . .
N13 C14 C15 122.5(3) . .
N13 C14 C14 117.03(18) . 2
C15 C14 C14 120.4(2) . 2
C16 C15 C14 117.9(3) . .
C16 C15 C19 123.0(3) . .
C14 C15 C19 119.1(3) . .
C17 C16 C15 119.8(3) . .
C17 C16 H16 120.1 . .
C15 C16 H16 120.1 . .
C16 C17 C18 118.0(4) . .
C16 C17 H17 121.0 . .
C18 C17 H17 121.0 . .
N13 C18 C17 124.3(3) . .
N13 C18 H18 117.9 . .
C17 C18 H18 117.9 . .
N20 C19 C19 121.5(2) . 2
N20 C19 C15 118.1(3) . .
C19 C19 C15 120.40(19) 2 .
N20 C21 C21 122.4(2) . 2
N20 C21 H21 118.8 . .
C21 C21 H21 118.8 2 .
N3 B2 N8 110.1(3) . .
N3 B2 H2A 109.6 . .
N8 B2 H2A 109.6 . .
N3 B2 H2B 109.6 . .
N8 B2 H2B 109.6 . .
H2A B2 H2B 108.2 . .
C27 N22 C23 116.3(3) . .
C33 N28 C29 117.2(4) . .
C37 N36 C35 116.4(4) . .
C38 N39 C34 115.4(4) . .
N22 C23 C24 122.9(3) . .
N22 C23 C29 117.3(3) . .
C24 C23 C29 119.8(3) . .
C23 C24 C25 118.4(4) . .
C23 C24 C34 120.1(3) . .
C25 C24 C34 121.6(4) . .
C26 C25 C24 118.9(4) . .
C26 C25 H25 120.6 . .
C24 C25 H25 120.6 . .
C25 C26 C27 119.1(4) . .
C25 C26 H26 120.5 . .
C27 C26 H26 120.5 . .
N22 C27 C26 124.4(4) . .
N22 C27 H27 117.8 . .
C26 C27 H27 117.8 . .
N28 C29 C30 122.7(3) . .
N28 C29 C23 117.6(3) . .
C30 C29 C23 119.6(3) . .
C31 C30 C29 117.9(4) . .
C31 C30 C35 122.0(4) . .
C29 C30 C35 120.1(3) . .
C32 C31 C30 119.4(4) . .
C32 C31 H31 120.3 . .
C30 C31 H31 120.3 . .
C31 C32 C33 118.8(4) . .
C31 C32 H32 120.6 . .
C33 C32 H32 120.6 . .
N28 C33 C32 124.0(5) . .
N28 C33 H33 118.0 . .
C32 C33 H33 118.0 . .
N39 C34 C35 122.4(4) . .
N39 C34 C24 117.7(4) . .
C35 C34 C24 119.9(3) . .
N36 C35 C34 120.6(4) . .
N36 C35 C30 118.9(4) . .
C34 C35 C30 120.5(3) . .
N36 C37 C38 122.7(4) . .
N36 C37 H37 118.6 . .
C38 C37 H37 118.6 . .
N39 C38 C37 122.4(5) . .
N39 C38 H38 118.8 . .
C37 C38 H38 118.8 . .
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 2.184(3) .
Fe1 N13 2.225(3) .
N3 C7 1.325(5) .
N3 N4 1.355(4) .
N3 B2 1.548(6) .
N4 C5 1.333(5) .
N8 C12 1.350(5) .
N8 N9 1.361(4) .
N8 B2 1.557(5) .
N9 C10 1.327(5) .
N13 C18 1.320(4) .
N13 C14 1.353(4) .
N20 C21 1.316(5) .
N20 C19 1.347(4) .
C5 C6 1.374(6) .
C5 H5 0.9300 .
C6 C7 1.376(6) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C10 C11 1.386(5) .
C10 H10 0.9300 .
C11 C12 1.356(6) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C14 C15 1.398(4) .
C14 C14 1.466(7) 2
C15 C16 1.394(5) .
C15 C19 1.465(5) .
C16 C17 1.369(5) .
C16 H16 0.9300 .
C17 C18 1.389(5) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 C19 1.398(7) 2
C21 C21 1.396(9) 2
C21 H21 0.9300 .
B2 H2A 0.9700 .
B2 H2B 0.9700 .
N22 C27 1.325(5) .
N22 C23 1.356(5) .
N28 C33 1.322(5) .
N28 C29 1.350(5) .
N36 C37 1.307(6) .
N36 C35 1.362(5) .
N39 C38 1.327(6) .
N39 C34 1.350(5) .
C23 C24 1.394(5) .
C23 C29 1.473(5) .
C24 C25 1.402(5) .
C24 C34 1.459(5) .
C25 C26 1.347(5) .
C25 H25 0.9300 .
C26 C27 1.394(5) .
C26 H26 0.9300 .
C27 H27 0.9300 .
C29 C30 1.400(5) .
C30 C31 1.393(5) .
C30 C35 1.445(5) .
C31 C32 1.359(6) .
C31 H31 0.9300 .
C32 C33 1.389(6) .
C32 H32 0.9300 .
C33 H33 0.9300 .
C34 C35 1.397(5) .
C37 C38 1.397(7) .
C37 H37 0.9300 .
C38 H38 0.9300 .
