#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:46:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179513 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/10/4341003.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_4341003
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                 118.923(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.325(2)
_cell_length_b                   14.0128(8)
_cell_length_c                   15.0338(11)
_cell_measurement_reflns_used    3143
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      24.75
_cell_measurement_theta_min      1.99
_cell_volume                     4854.1(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      220(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.842
_diffrn_measured_fraction_theta_max 0.842
_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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0955
_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            14049
_diffrn_reflns_theta_full        29.80
_diffrn_reflns_theta_max         29.80
_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    0.374
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.844
_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    1.432
_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         -0.414
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0675
_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)+(0.0610P)²+2.0425P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1670
_reflns_number_gt                3611
_reflns_number_total             5858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501402q_si_003.cif
_cod_data_source_block           rk14a220
_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        4854.0(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4341003
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 0.26299(4) 0.2500 0.02645(19) Uani 1 2 d S
N3 N -0.12630(10) 0.30374(19) 0.0723(2) 0.0355(6) Uani 1 1 d .
N4 N -0.07284(10) 0.26944(17) 0.0959(2) 0.0315(6) Uani 1 1 d .
N8 N -0.10264(10) 0.38658(17) 0.2381(2) 0.0333(6) Uani 1 1 d .
N9 N -0.04438(10) 0.36842(16) 0.2912(2) 0.0314(6) Uani 1 1 d .
N13 N -0.03059(10) 0.13748(16) 0.30022(19) 0.0289(6) Uani 1 1 d .
N20 N -0.03338(11) -0.20687(18) 0.3001(2) 0.0414(7) Uani 1 1 d .
C5 C -0.07335(14) 0.2581(2) 0.0070(3) 0.0364(8) Uani 1 1 d .
H5 H -0.0418 0.2350 0.0005 0.044 Uiso 1 1 calc R
C6 C -0.12582(15) 0.2844(3) -0.0735(3) 0.0458(9) Uani 1 1 d .
H6 H -0.1370 0.2834 -0.1430 0.055 Uiso 1 1 calc R
C7 C -0.15834(14) 0.3126(3) -0.0284(3) 0.0496(9) Uani 1 1 d .
H7 H -0.1969 0.3345 -0.0631 0.059 Uiso 1 1 calc R
C10 C -0.02112(14) 0.4380(2) 0.3597(3) 0.0372(8) Uani 1 1 d .
H10 H 0.0187 0.4437 0.4060 0.045 Uiso 1 1 calc R
C11 C -0.06346(16) 0.5011(2) 0.3538(3) 0.0443(9) Uani 1 1 d .
H11 H -0.0585 0.5555 0.3938 0.053 Uiso 1 1 calc R
C12 C -0.11395(16) 0.4658(2) 0.2763(3) 0.0430(9) Uani 1 1 d .
H12 H -0.1509 0.4927 0.2532 0.052 Uiso 1 1 calc R
C14 C -0.01649(11) 0.05084(19) 0.2777(2) 0.0249(6) Uani 1 1 d .
C15 C -0.03204(12) -0.0349(2) 0.3047(2) 0.0293(7) Uani 1 1 d .
C16 C -0.06258(12) -0.0303(2) 0.3595(3) 0.0371(8) Uani 1 1 d .
H16 H -0.0738 -0.0867 0.3791 0.045 Uiso 1 1 calc R
C17 C -0.07587(13) 0.0566(2) 0.3842(3) 0.0372(8) Uani 1 1 d .
H17 H -0.0957 0.0608 0.4219 0.045 Uiso 1 1 calc R
C18 C -0.05955(13) 0.1385(2) 0.3523(2) 0.0347(7) Uani 1 1 d .
H18 H -0.0695 0.1980 0.3685 0.042 Uiso 1 1 calc R
C19 C -0.01602(12) -0.12466(19) 0.2758(2) 0.0315(7) Uani 1 1 d .
C21 C -0.01702(15) -0.2863(2) 0.2742(3) 0.0479(9) Uani 1 1 d .
H21 H -0.0286 -0.3451 0.2887 0.057 Uiso 1 1 calc R
B2 B -0.14527(15) 0.3185(3) 0.1546(3) 0.0407(9) Uani 1 1 d .
H2A H -0.1845 0.3455 0.1232 0.049 Uiso 1 1 calc R
H2B H -0.1459 0.2569 0.1849 0.049 Uiso 1 1 calc R
N22 N -0.10874(11) -0.24088(18) 0.0090(2) 0.0358(6) Uani 1 1 d .
N28 N -0.13385(11) -0.05888(18) 0.0389(2) 0.0413(7) Uani 1 1 d .
N36 N -0.24712(12) -0.1765(2) 0.1893(2) 0.0505(8) Uani 1 1 d .
N39 N -0.22458(11) -0.3651(2) 0.1522(2) 0.0434(7) Uani 1 1 d .
C23 C -0.14265(12) -0.2290(2) 0.0532(2) 0.0293(7) Uani 1 1 d .
C24 C -0.16609(12) -0.3057(2) 0.0808(2) 0.0314(7) Uani 1 1 d .
C25 C -0.15480(13) -0.3989(2) 0.0597(2) 0.0368(8) Uani 1 1 d .
H25 H -0.1702 -0.4521 0.0765 0.044 Uiso 1 1 calc R
C26 C -0.12124(14) -0.4108(2) 0.0146(3) 0.0423(8) Uani 1 1 d .
H26 H -0.1132 -0.4722 -0.0005 0.051 Uiso 1 1 calc R
C27 C -0.09907(13) -0.3303(2) -0.0088(3) 0.0416(8) Uani 1 1 d .
H27 H -0.0756 -0.3397 -0.0393 0.050 Uiso 1 1 calc R
C29 C -0.15560(12) -0.1307(2) 0.0698(2) 0.0307(7) Uani 1 1 d .
C30 C -0.19114(12) -0.1150(2) 0.1148(2) 0.0354(8) Uani 1 1 d .
C31 C -0.20482(15) -0.0209(3) 0.1247(3) 0.0490(9) Uani 1 1 d .
H31 H -0.2286 -0.0076 0.1539 0.059 Uiso 1 1 calc R
C32 C -0.18367(16) 0.0521(3) 0.0918(3) 0.0574(11) Uani 1 1 d .
H32 H -0.1929 0.1159 0.0971 0.069 Uiso 1 1 calc R
C33 C -0.14812(16) 0.0296(2) 0.0503(3) 0.0526(10) Uani 1 1 d .
H33 H -0.1332 0.0802 0.0288 0.063 Uiso 1 1 calc R
C34 C -0.20230(12) -0.2884(2) 0.1278(2) 0.0349(7) Uani 1 1 d .
C35 C -0.21379(12) -0.1945(2) 0.1457(2) 0.0367(8) Uani 1 1 d .
C37 C -0.26853(15) -0.2514(3) 0.2124(3) 0.0552(11) Uani 1 1 d .
H37 H -0.2918 -0.2416 0.2431 0.066 Uiso 1 1 calc R
C38 C -0.25818(14) -0.3448(3) 0.1932(3) 0.0544(10) Uani 1 1 d .
H38 H -0.2756 -0.3953 0.2099 0.065 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 93.28(12) . 2
N9 Fe1 N4 89.25(9) . 2
N9 Fe1 N4 87.49(9) . .
N4 Fe1 N4 175.25(13) 2 .
N9 Fe1 N13 168.91(8) . 2
N4 Fe1 N13 87.06(9) . 2
N9 Fe1 N13 96.30(9) . .
N4 Fe1 N13 96.73(9) . .
N13 Fe1 N13 74.77(12) 2 .
C7 N3 N4 109.5(3) . .
C7 N3 B2 128.3(3) . .
N4 N3 B2 121.9(3) . .
C5 N4 N3 105.8(3) . .
C5 N4 Fe1 129.4(2) . .
N3 N4 Fe1 123.92(19) . .
C12 N8 N9 108.7(3) . .
C12 N8 B2 129.2(3) . .
N9 N8 B2 121.9(2) . .
C10 N9 N8 106.3(2) . .
C10 N9 Fe1 127.9(2) . .
N8 N9 Fe1 124.87(18) . .
C18 N13 C14 117.3(2) . .
C18 N13 Fe1 126.7(2) . .
C14 N13 Fe1 115.91(18) . .
C21 N20 C19 115.9(3) . .
N4 C5 C6 111.5(3) . .
N4 C5 H5 124.2 . .
C6 C5 H5 124.2 . .
C5 C6 C7 104.0(3) . .
C5 C6 H6 128.0 . .
C7 C6 H6 128.0 . .
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 104.1(3) . .
C12 C11 H11 128.0 . .
C10 C11 H11 128.0 . .
N8 C12 C11 109.7(3) . .
N8 C12 H12 125.2 . .
C11 C12 H12 125.2 . .
N13 C14 C15 123.0(3) . .
N13 C14 C14 116.71(15) . 2
C15 C14 C14 120.28(16) . 2
C14 C15 C16 117.7(3) . .
C14 C15 C19 119.4(3) . .
C16 C15 C19 123.0(3) . .
C17 C16 C15 119.6(3) . .
C17 C16 H16 120.2 . .
C15 C16 H16 120.2 . .
C16 C17 C18 118.7(3) . .
C16 C17 H17 120.6 . .
C18 C17 H17 120.6 . .
N13 C18 C17 123.6(3) . .
N13 C18 H18 118.2 . .
C17 C18 H18 118.2 . .
N20 C19 C19 121.61(18) . 2
N20 C19 C15 118.0(3) . .
C19 C19 C15 120.34(16) 2 .
N20 C21 C21 122.41(19) . 2
N20 C21 H21 118.8 . .
C21 C21 H21 118.8 2 .
N8 B2 N3 110.0(3) . .
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 116.7(3) . .
C33 N28 C29 117.2(3) . .
C37 N36 C35 116.2(3) . .
C38 N39 C34 115.3(3) . .
N22 C23 C24 122.7(3) . .
N22 C23 C29 117.4(3) . .
C24 C23 C29 119.9(3) . .
C23 C24 C25 118.3(3) . .
C23 C24 C34 120.2(3) . .
C25 C24 C34 121.5(3) . .
C26 C25 C24 119.0(3) . .
C26 C25 H25 120.5 . .
C24 C25 H25 120.5 . .
C25 C26 C27 118.7(3) . .
C25 C26 H26 120.6 . .
C27 C26 H26 120.6 . .
N22 C27 C26 124.6(3) . .
N22 C27 H27 117.7 . .
C26 C27 H27 117.7 . .
N28 C29 C30 122.7(3) . .
N28 C29 C23 118.0(3) . .
C30 C29 C23 119.2(3) . .
C31 C30 C29 117.6(3) . .
C31 C30 C35 121.9(3) . .
C29 C30 C35 120.5(3) . .
C32 C31 C30 119.9(3) . .
C32 C31 H31 120.1 . .
C30 C31 H31 120.1 . .
C31 C32 C33 118.2(3) . .
C31 C32 H32 120.9 . .
C33 C32 H32 120.9 . .
N28 C33 C32 124.3(4) . .
N28 C33 H33 117.9 . .
C32 C33 H33 117.9 . .
N39 C34 C35 121.9(3) . .
N39 C34 C24 118.0(3) . .
C35 C34 C24 120.1(3) . .
N36 C35 C34 121.2(3) . .
N36 C35 C30 118.7(3) . .
C34 C35 C30 120.1(3) . .
N36 C37 C38 122.9(3) . .
N36 C37 H37 118.6 . .
C38 C37 H37 118.6 . .
N39 C38 C37 122.4(3) . .
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 2.152(2) .
Fe1 N4 2.181(3) .
Fe1 N13 2.214(2) .
N3 C7 1.336(4) .
N3 N4 1.362(3) .
N3 B2 1.556(5) .
N4 C5 1.339(4) .
N8 C12 1.348(4) .
N8 N9 1.367(3) .
N8 B2 1.543(5) .
N9 C10 1.333(4) .
N13 C18 1.332(4) .
N13 C14 1.359(3) .
N20 C21 1.319(4) .
N20 C19 1.353(4) .
C5 C6 1.375(5) .
C5 H5 0.9400 .
C6 C7 1.381(5) .
C6 H6 0.9400 .
C7 H7 0.9400 .
C10 C11 1.391(4) .
C10 H10 0.9400 .
C11 C12 1.367(5) .
C11 H11 0.9400 .
C12 H12 0.9400 .
C14 C15 1.391(4) .
C14 C14 1.466(5) 2
C15 C16 1.403(4) .
C15 C19 1.458(4) .
C16 C17 1.366(4) .
C16 H16 0.9400 .
C17 C18 1.390(4) .
C17 H17 0.9400 .
C18 H18 0.9400 .
C19 C19 1.395(6) 2
C21 C21 1.400(7) 2
C21 H21 0.9400 .
B2 H2A 0.9800 .
B2 H2B 0.9800 .
N22 C27 1.331(4) .
N22 C23 1.356(4) .
N28 C33 1.330(4) .
N28 C29 1.346(4) .
N36 C37 1.314(5) .
N36 C35 1.349(4) .
N39 C38 1.331(4) .
N39 C34 1.357(4) .
C23 C24 1.399(4) .
C23 C29 1.470(4) .
C24 C25 1.409(4) .
C24 C34 1.456(4) .
C25 C26 1.359(4) .
C25 H25 0.9400 .
C26 C27 1.391(4) .
C26 H26 0.9400 .
C27 H27 0.9400 .
C29 C30 1.412(4) .
C30 C31 1.395(4) .
C30 C35 1.442(5) .
C31 C32 1.367(5) .
C31 H31 0.9400 .
C32 C33 1.389(5) .
C32 H32 0.9400 .
C33 H33 0.9400 .
C34 C35 1.405(5) .
C37 C38 1.395(5) .
C37 H37 0.9400 .
C38 H38 0.9400 .
