#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:46:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179513 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/10/4341002.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_4341002
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                 118.981(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.3126(19)
_cell_length_b                   13.9971(8)
_cell_length_c                   15.0236(10)
_cell_measurement_reflns_used    3256
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.79
_cell_measurement_theta_min      2.00
_cell_volume                     4840.3(6)
_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      200(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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0893
_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            14000
_diffrn_reflns_theta_full        29.82
_diffrn_reflns_theta_max         29.82
_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    0.375
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.829
_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    1.436
_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         0.816
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0654
_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)+(0.0647P)²+0.3924P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1617
_reflns_number_gt                3773
_reflns_number_total             5850
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501402q_si_003.cif
_cod_data_source_block           rk14a200
_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        4840.3(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4341002
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 0.26300(4) 0.2500 0.02380(18) Uani 1 2 d S
N3 N -0.12622(9) 0.30361(17) 0.07245(19) 0.0319(6) Uani 1 1 d .
N4 N -0.07280(9) 0.26928(16) 0.09586(19) 0.0285(5) Uani 1 1 d .
N8 N -0.10248(10) 0.38673(16) 0.23842(19) 0.0300(6) Uani 1 1 d .
N9 N -0.04428(9) 0.36863(15) 0.29101(19) 0.0292(6) Uani 1 1 d .
N13 N -0.03080(9) 0.13765(16) 0.29980(18) 0.0272(5) Uani 1 1 d .
N20 N -0.03343(10) -0.20677(17) 0.3002(2) 0.0371(6) Uani 1 1 d .
C5 C -0.07324(13) 0.2580(2) 0.0071(2) 0.0352(7) Uani 1 1 d .
H5 H -0.0412 0.2350 0.0007 0.042 Uiso 1 1 calc R
C6 C -0.12591(13) 0.2837(2) -0.0738(3) 0.0410(8) Uani 1 1 d .
H6 H -0.1373 0.2822 -0.1442 0.049 Uiso 1 1 calc R
C7 C -0.15841(13) 0.3122(2) -0.0287(3) 0.0439(8) Uani 1 1 d .
H7 H -0.1974 0.3344 -0.0638 0.053 Uiso 1 1 calc R
C10 C -0.02097(14) 0.4385(2) 0.3597(3) 0.0365(7) Uani 1 1 d .
H10 H 0.0193 0.4444 0.4064 0.044 Uiso 1 1 calc R
C11 C -0.06298(15) 0.5009(2) 0.3541(3) 0.0414(8) Uani 1 1 d .
H11 H -0.0578 0.5558 0.3948 0.050 Uiso 1 1 calc R
C12 C -0.11377(15) 0.4661(2) 0.2767(3) 0.0393(8) Uani 1 1 d .
H12 H -0.1511 0.4935 0.2535 0.047 Uiso 1 1 calc R
C14 C -0.01663(10) 0.05151(18) 0.2775(2) 0.0233(6) Uani 1 1 d .
C15 C -0.03226(11) -0.03465(19) 0.3046(2) 0.0274(6) Uani 1 1 d .
C16 C -0.06273(12) -0.0305(2) 0.3593(2) 0.0332(7) Uani 1 1 d .
H16 H -0.0741 -0.0876 0.3791 0.040 Uiso 1 1 calc R
C17 C -0.07604(12) 0.0572(2) 0.3839(2) 0.0361(7) Uani 1 1 d .
H17 H -0.0958 0.0618 0.4225 0.043 Uiso 1 1 calc R
C18 C -0.05993(12) 0.1389(2) 0.3514(2) 0.0308(7) Uani 1 1 d .
H18 H -0.0703 0.1992 0.3669 0.037 Uiso 1 1 calc R
C19 C -0.01590(11) -0.12469(18) 0.2763(2) 0.0292(6) Uani 1 1 d .
C21 C -0.01709(13) -0.2864(2) 0.2739(3) 0.0425(8) Uani 1 1 d .
H21 H -0.0290 -0.3459 0.2881 0.051 Uiso 1 1 calc R
B2 B -0.14536(14) 0.3189(3) 0.1542(3) 0.0363(9) Uani 1 1 d .
H2A H -0.1849 0.3467 0.1221 0.044 Uiso 1 1 calc R
H2B H -0.1465 0.2567 0.1845 0.044 Uiso 1 1 calc R
N22 N -0.10858(10) -0.24126(16) 0.0090(2) 0.0326(6) Uani 1 1 d .
N28 N -0.13397(10) -0.05877(17) 0.0384(2) 0.0371(6) Uani 1 1 d .
N36 N -0.24725(11) -0.1765(2) 0.1892(2) 0.0454(7) Uani 1 1 d .
N39 N -0.22464(10) -0.36558(19) 0.1523(2) 0.0387(6) Uani 1 1 d .
C23 C -0.14261(11) -0.2291(2) 0.0532(2) 0.0281(6) Uani 1 1 d .
C24 C -0.16597(11) -0.3061(2) 0.0809(2) 0.0284(6) Uani 1 1 d .
C25 C -0.15480(12) -0.3994(2) 0.0595(2) 0.0334(7) Uani 1 1 d .
H25 H -0.1705 -0.4533 0.0762 0.040 Uiso 1 1 calc R
C26 C -0.12138(13) -0.4109(2) 0.0147(3) 0.0384(8) Uani 1 1 d .
H26 H -0.1134 -0.4730 -0.0010 0.046 Uiso 1 1 calc R
C27 C -0.09876(12) -0.3303(2) -0.0084(3) 0.0372(8) Uani 1 1 d .
H27 H -0.0747 -0.3399 -0.0385 0.045 Uiso 1 1 calc R
C29 C -0.15548(11) -0.13064(19) 0.0697(2) 0.0271(6) Uani 1 1 d .
C30 C -0.19124(12) -0.1152(2) 0.1147(2) 0.0330(7) Uani 1 1 d .
C31 C -0.20507(13) -0.0204(2) 0.1240(3) 0.0443(9) Uani 1 1 d .
H31 H -0.2293 -0.0070 0.1531 0.053 Uiso 1 1 calc R
C32 C -0.18394(15) 0.0522(2) 0.0916(3) 0.0527(10) Uani 1 1 d .
H32 H -0.1934 0.1167 0.0969 0.063 Uiso 1 1 calc R
C33 C -0.14795(14) 0.0301(2) 0.0502(3) 0.0474(9) Uani 1 1 d .
H33 H -0.1325 0.0814 0.0293 0.057 Uiso 1 1 calc R
C34 C -0.20212(11) -0.2892(2) 0.1280(2) 0.0305(7) Uani 1 1 d .
C35 C -0.21393(11) -0.1952(2) 0.1454(2) 0.0335(7) Uani 1 1 d .
C37 C -0.26888(14) -0.2520(3) 0.2119(3) 0.0498(10) Uani 1 1 d .
H37 H -0.2927 -0.2422 0.2425 0.060 Uiso 1 1 calc R
C38 C -0.25833(13) -0.3448(3) 0.1930(3) 0.0486(9) Uani 1 1 d .
H38 H -0.2759 -0.3958 0.2100 0.058 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 93.06(12) 2 .
N9 Fe1 N4 87.56(9) . .
N9 Fe1 N4 89.26(9) . 2
N4 Fe1 N4 175.37(12) . 2
N9 Fe1 N13 96.34(8) . .
N4 Fe1 N13 96.56(8) . .
N9 Fe1 N13 169.14(8) . 2
N4 Fe1 N13 87.13(9) . 2
N13 Fe1 N13 74.88(11) . 2
C7 N3 N4 109.4(2) . .
C7 N3 B2 128.0(3) . .
N4 N3 B2 122.4(2) . .
C5 N4 N3 106.0(2) . .
C5 N4 Fe1 129.3(2) . .
N3 N4 Fe1 123.74(18) . .
C12 N8 N9 108.9(2) . .
C12 N8 B2 129.1(2) . .
N9 N8 B2 122.0(2) . .
C10 N9 N8 106.1(2) . .
C10 N9 Fe1 127.99(19) . .
N8 N9 Fe1 125.03(17) . .
C18 N13 C14 117.6(2) . .
C18 N13 Fe1 126.65(19) . .
C14 N13 Fe1 115.69(17) . .
C21 N20 C19 115.8(3) . .
N4 C5 C6 111.6(3) . .
N4 C5 H5 124.2 . .
C6 C5 H5 124.2 . .
C5 C6 C7 103.9(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 104.5(3) . .
C12 C11 H11 127.8 . .
C10 C11 H11 127.8 . .
N8 C12 C11 109.2(3) . .
N8 C12 H12 125.4 . .
C11 C12 H12 125.4 . .
N13 C14 C15 122.8(2) . .
N13 C14 C14 116.87(14) . 2
C15 C14 C14 120.31(16) . 2
C14 C15 C16 117.9(3) . .
C14 C15 C19 119.4(2) . .
C16 C15 C19 122.7(2) . .
C17 C16 C15 119.2(3) . .
C17 C16 H16 120.4 . .
C15 C16 H16 120.4 . .
C16 C17 C18 118.6(3) . .
C16 C17 H17 120.7 . .
C18 C17 H17 120.7 . .
N13 C18 C17 123.7(3) . .
N13 C18 H18 118.1 . .
C17 C18 H18 118.1 . .
N20 C19 C19 121.60(17) . 2
N20 C19 C15 118.1(3) . .
C19 C19 C15 120.29(15) 2 .
N20 C21 C21 122.50(18) . 2
N20 C21 H21 118.7 . .
C21 C21 H21 118.7 2 .
N8 B2 N3 110.2(2) . .
N8 B2 H2A 109.6 . .
N3 B2 H2A 109.6 . .
N8 B2 H2B 109.6 . .
N3 B2 H2B 109.6 . .
H2A B2 H2B 108.1 . .
C27 N22 C23 116.9(3) . .
C33 N28 C29 117.4(3) . .
C37 N36 C35 115.7(3) . .
C38 N39 C34 115.3(3) . .
N22 C23 C24 122.5(3) . .
N22 C23 C29 117.5(2) . .
C24 C23 C29 120.1(2) . .
C23 C24 C25 118.3(3) . .
C23 C24 C34 120.3(3) . .
C25 C24 C34 121.3(3) . .
C26 C25 C24 118.8(3) . .
C26 C25 H25 120.6 . .
C24 C25 H25 120.6 . .
C25 C26 C27 119.1(3) . .
C25 C26 H26 120.5 . .
C27 C26 H26 120.5 . .
N22 C27 C26 124.4(3) . .
N22 C27 H27 117.8 . .
C26 C27 H27 117.8 . .
N28 C29 C30 122.9(3) . .
N28 C29 C23 118.1(2) . .
C30 C29 C23 119.0(3) . .
C31 C30 C29 117.2(3) . .
C31 C30 C35 122.3(3) . .
C29 C30 C35 120.5(3) . .
C32 C31 C30 120.2(3) . .
C32 C31 H31 119.9 . .
C30 C31 H31 119.9 . .
C31 C32 C33 118.5(3) . .
C31 C32 H32 120.7 . .
C33 C32 H32 120.7 . .
N28 C33 C32 123.9(3) . .
N28 C33 H33 118.1 . .
C32 C33 H33 118.1 . .
N39 C34 C35 121.6(3) . .
N39 C34 C24 118.5(3) . .
C35 C34 C24 119.9(3) . .
N36 C35 C34 121.7(3) . .
N36 C35 C30 118.1(3) . .
C34 C35 C30 120.2(3) . .
N36 C37 C38 122.8(3) . .
N36 C37 H37 118.6 . .
C38 C37 H37 118.6 . .
N39 C38 C37 122.9(3) . .
N39 C38 H38 118.6 . .
C37 C38 H38 118.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N9 2.149(2) .
Fe1 N4 2.177(2) .
Fe1 N13 2.210(2) .
N3 C7 1.339(4) .
N3 N4 1.361(3) .
N3 B2 1.552(4) .
N4 C5 1.337(4) .
N8 C12 1.349(4) .
N8 N9 1.364(3) .
N8 B2 1.546(4) .
N9 C10 1.336(4) .
N13 C18 1.328(3) .
N13 C14 1.352(3) .
N20 C21 1.322(4) .
N20 C19 1.350(3) .
C5 C6 1.377(4) .
C5 H5 0.9500 .
C6 C7 1.383(4) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C10 C11 1.379(4) .
C10 H10 0.9500 .
C11 C12 1.368(4) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C14 C15 1.397(4) .
C14 C14 1.465(5) 2
C15 C16 1.400(4) .
C15 C19 1.460(4) .
C16 C17 1.377(4) .
C16 H16 0.9500 .
C17 C18 1.388(4) .
C17 H17 0.9500 .
C18 H18 0.9500 .
C19 C19 1.402(6) 2
C21 C21 1.397(7) 2
C21 H21 0.9500 .
B2 H2A 0.9900 .
B2 H2B 0.9900 .
N22 C27 1.324(4) .
N22 C23 1.359(3) .
N28 C33 1.333(4) .
N28 C29 1.346(4) .
N36 C37 1.320(4) .
N36 C35 1.352(4) .
N39 C38 1.331(4) .
N39 C34 1.355(4) .
C23 C24 1.401(4) .
C23 C29 1.469(4) .
C24 C25 1.410(4) .
C24 C34 1.454(4) .
C25 C26 1.351(4) .
C25 H25 0.9500 .
C26 C27 1.395(4) .
C26 H26 0.9500 .
C27 H27 0.9500 .
C29 C30 1.416(4) .
C30 C31 1.400(4) .
C30 C35 1.445(4) .
C31 C32 1.358(5) .
C31 H31 0.9500 .
C32 C33 1.396(5) .
C32 H32 0.9500 .
C33 H33 0.9500 .
C34 C35 1.405(4) .
C37 C38 1.387(5) .
C37 H37 0.9500 .
C38 H38 0.9500 .
