#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/38/4123891.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_4123891
loop_
_publ_author_name
'Pinkowicz, Dawid'
'Rams, Michał'
'Mišek, Martin'
'Kamenev, Konstantin V.'
'Tomkowiak, Hanna'
'Katrusiak, Andrzej'
'Sieklucka, Barbara'
_publ_section_title
;
 Enforcing Multifunctionality: A Pressure-Induced Spin-Crossover
 Photomagnet.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8795
_journal_page_last               8802
_journal_paper_doi               10.1021/jacs.5b04303
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb,4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.7080(16)
_cell_length_b                   21.7080(16)
_cell_length_c                   9.636(2)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      4.20
_cell_volume                     4540.8(11)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction, 2002)'
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2002)'
_computing_molecular_graphics
;
Mercury
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Kuma KM4CCD κ geometry'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.5132
_diffrn_reflns_av_sigmaI/netI    0.2010
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            102331
_diffrn_reflns_theta_full        27.71
_diffrn_reflns_theta_max         27.71
_diffrn_reflns_theta_min         4.20
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;   
Xcalibur CCD System, CrysAlisPro Software System, version 171.37.31;
 Oxford Diffraction Poland, 2014 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.348
_refine_diff_density_min         -5.326
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2566
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.2611
_refine_ls_R_factor_gt           0.2243
_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)+(0.3665P)²+427.5840P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5596
_refine_ls_wR_factor_ref         0.5753
_reflns_number_gt                2092
_reflns_number_total             2566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b04303_si_002.cif
_cod_data_source_block           5.00a
_cod_depositor_comments
'Adding full bibliography for 4123890--4123892.cif.'
_cod_original_cell_volume        4540.7(11)
_cod_original_sg_symbol_H-M      I41/a
_cod_database_code               4123891
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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
Nb1 Nb 0.5000 0.7500 0.6250 0.0009(9) Uani 1 4 d SU
Fe Fe 0.5000 1.0000 0.5000 0.0455(16) Uani 1 2 d SU
N1 N 0.4855(10) 0.9014(9) 0.520(2) 0.039(5) Uani 1 1 d U
C2 C 0.5584(11) 0.7593(12) 0.439(3) 0.039(6) Uani 1 1 d U
N2 N 0.5869(10) 0.7655(11) 0.336(2) 0.046(5) Uani 1 1 d U
C1 C 0.4877(12) 0.8497(12) 0.554(3) 0.040(6) Uani 1 1 d U
N22 N 0.5484(10) 1.0359(10) 0.205(2) 0.041(5) Uani 1 1 d U
H22 H 0.5375 1.0733 0.2208 0.049 Uiso 1 1 calc R
N21 N 0.5450(10) 0.9884(9) 0.297(2) 0.040(5) Uani 1 1 d U
C25 C 0.5691(13) 0.9436(13) 0.232(3) 0.050(7) Uani 1 1 d U
H25 H 0.5765 0.9053 0.2720 0.060 Uiso 1 1 calc R
C24 C 0.5831(19) 0.9580(19) 0.096(4) 0.084(11) Uani 1 1 d U
H24 H 0.5980 0.9317 0.0277 0.101 Uiso 1 1 calc R
C23 C 0.5711(17) 1.0150(18) 0.086(4) 0.072(10) Uani 1 1 d U
H23 H 0.5773 1.0386 0.0066 0.086 Uiso 1 1 calc R
N11 N 0.5859(10) 0.9864(10) 0.611(2) 0.044(5) Uani 1 1 d U
N12 N 0.6252(13) 0.9390(12) 0.600(3) 0.063(7) Uani 1 1 d U
H12 H 0.6227 0.9081 0.5439 0.076 Uiso 1 1 calc R
C15 C 0.6080(10) 1.0222(11) 0.709(2) 0.031(5) Uani 1 1 d U
H15 H 0.5883 1.0581 0.7378 0.037 Uiso 1 1 calc R
C14 C 0.6597(16) 1.0032(16) 0.763(4) 0.066(9) Uani 1 1 d U
H14 H 0.6832 1.0224 0.8308 0.079 Uiso 1 1 calc R
C13 C 0.6713(15) 0.9509(15) 0.699(4) 0.060(8) Uani 1 1 d U
H13 H 0.7050 0.9256 0.7169 0.072 Uiso 1 1 calc R
O1 O 0.5599(9) 0.6334(9) 0.192(2) 0.051(5) Uani 1 1 d DU
H1A H 0.602(2) 0.640(9) 0.18(3) 0.061 Uiso 1 1 d D
H1B H 0.529(6) 0.663(7) 0.20(3) 0.061 Uiso 1 1 d D
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'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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
C2 Nb1 C2 71.1(13) 12_767 15_566
C2 Nb1 C2 131.5(8) 12_767 .
C2 Nb1 C2 131.5(8) 15_566 .
C2 Nb1 C2 131.5(8) 12_767 6_564
C2 Nb1 C2 131.5(8) 15_566 6_564
C2 Nb1 C2 71.1(13) . 6_564
C2 Nb1 C1 77.1(9) 12_767 15_566
C2 Nb1 C1 74.8(9) 15_566 15_566
C2 Nb1 C1 71.9(9) . 15_566
C2 Nb1 C1 142.9(9) 6_564 15_566
C2 Nb1 C1 142.9(9) 12_767 6_564
C2 Nb1 C1 71.9(9) 15_566 6_564
C2 Nb1 C1 77.1(9) . 6_564
C2 Nb1 C1 74.8(9) 6_564 6_564
C1 Nb1 C1 95.1(4) 15_566 6_564
C2 Nb1 C1 74.8(9) 12_767 12_767
C2 Nb1 C1 77.1(9) 15_566 12_767
C2 Nb1 C1 142.9(9) . 12_767
C2 Nb1 C1 71.9(9) 6_564 12_767
C1 Nb1 C1 145.2(13) 15_566 12_767
C1 Nb1 C1 95.1(4) 6_564 12_767
C2 Nb1 C1 71.9(9) 12_767 .
C2 Nb1 C1 142.9(9) 15_566 .
C2 Nb1 C1 74.8(9) . .
C2 Nb1 C1 77.1(9) 6_564 .
C1 Nb1 C1 95.1(4) 15_566 .
C1 Nb1 C1 145.2(13) 6_564 .
C1 Nb1 C1 95.1(4) 12_767 .
N11 Fe N11 180.000(4) 9_676 .
N11 Fe N21 92.4(8) 9_676 9_676
N11 Fe N21 87.6(8) . 9_676
N11 Fe N21 87.6(8) 9_676 .
N11 Fe N21 92.4(8) . .
N21 Fe N21 180.000(5) 9_676 .
N11 Fe N1 87.0(8) 9_676 9_676
N11 Fe N1 93.0(8) . 9_676
N21 Fe N1 91.7(8) 9_676 9_676
N21 Fe N1 88.3(8) . 9_676
N11 Fe N1 93.0(8) 9_676 .
N11 Fe N1 87.0(8) . .
N21 Fe N1 88.3(8) 9_676 .
N21 Fe N1 91.7(8) . .
N1 Fe N1 180.000(3) 9_676 .
C1 N1 Fe 165(2) . .
N2 C2 Nb1 177(2) . .
N1 C1 Nb1 175(2) . .
C23 N22 N21 109(2) . .
C25 N21 N22 104(2) . .
C25 N21 Fe 135.0(19) . .
N22 N21 Fe 121.2(15) . .
N21 C25 C24 113(3) . .
C23 C24 C25 104(4) . .
C24 C23 N22 110(4) . .
C15 N11 N12 106(2) . .
C15 N11 Fe 126.0(16) . .
N12 N11 Fe 127.6(18) . .
N11 N12 C13 105(3) . .
C14 C15 N11 114(2) . .
C15 C14 C13 105(3) . .
C14 C13 N12 110(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 C2 2.21(3) 12_767
Nb1 C2 2.21(3) 15_566
Nb1 C2 2.21(3) .
Nb1 C2 2.21(3) 6_564
Nb1 C1 2.29(2) 15_566
Nb1 C1 2.29(2) 6_564
Nb1 C1 2.29(2) 12_767
Nb1 C1 2.29(2) .
Fe N11 2.17(2) 9_676
Fe N11 2.17(2) .
Fe N21 2.20(2) 9_676
Fe N21 2.20(2) .
Fe N1 2.17(2) 9_676
Fe N1 2.17(2) .
N1 C1 1.17(3) .
C2 N2 1.17(3) .
N22 C23 1.33(4) .
N22 N21 1.36(3) .
N21 C25 1.27(3) .
C25 C24 1.38(5) .
C24 C23 1.27(5) .
N11 C15 1.31(3) .
N11 N12 1.34(3) .
N12 C13 1.41(4) .
C15 C14 1.30(4) .
C14 C13 1.31(5) .
