#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/42/4124226.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_4124226
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                   20.717(2)
_cell_length_b                   20.717(2)
_cell_length_c                   9.222(6)
_cell_measurement_pressure       1870000
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.07
_cell_measurement_theta_min      3.69
_cell_volume                     3958(3)
_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 0.475
_diffrn_measured_fraction_theta_max 0.475
_diffrn_measurement_device_type  'Kuma KM4CCD κ geometry'
_diffrn_measurement_method
;
HP omega scans - for more details see:
A. Budzianowski, A. Katrusiak in High-Pressure Crystallography
(Eds.: A. Katrusiak, P. F. McMillan),
Dordrecht: Kluwer Acad. Publ., 2004 pp.157-168
;
_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  0.2007
_diffrn_reflns_av_sigmaI/netI    0.1738
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            9161
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.792
_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    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1143
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.2107
_refine_ls_R_factor_gt           0.0758
_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)+(0.0800P)²+5.1000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.2195
_reflns_number_gt                429
_reflns_number_total             1143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b04303_si_004.cif
_cod_data_source_block           1.87_GPa
_cod_original_cell_volume        3958(2)
_cod_original_sg_symbol_H-M      I41/a
_cod_database_code               4124226
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
Nb Nb 0.5000 0.7500 0.6250 0.0691(14) Uani 1 4 d SU
Fe Fe 0.2500 0.7500 0.7500 0.0697(15) Uani 1 2 d SU
C1 C 0.3988(6) 0.7664(5) 0.6936(18) 0.063(4) Uani 1 1 d U
N1 N 0.3453(5) 0.7702(4) 0.7309(15) 0.069(4) Uani 1 1 d U
C2 C 0.5601(7) 0.7397(7) 0.427(3) 0.083(5) Uani 1 1 d U
N2 N 0.5903(5) 0.7326(5) 0.3242(19) 0.076(4) Uani 1 1 d U
N11 N 0.2292(5) 0.8334(5) 0.8595(15) 0.067(4) Uani 1 1 d U
N12 N 0.2686(5) 0.8627(6) 0.9586(18) 0.087(4) Uani 1 1 d U
H12 H 0.3038 0.8455 0.9898 0.105 Uiso 1 1 calc R
C13 C 0.2474(7) 0.9206(7) 1.0028(19) 0.077(5) Uani 1 1 d U
H13 H 0.2667 0.9485 1.0689 0.093 Uiso 1 1 calc R
C14 C 0.1906(7) 0.9295(7) 0.928(2) 0.085(5) Uani 1 1 d U
H14 H 0.1633 0.9651 0.9308 0.102 Uiso 1 1 calc R
C15 C 0.1834(6) 0.8759(7) 0.852(2) 0.076(4) Uani 1 1 d U
H15 H 0.1469 0.8690 0.7951 0.091 Uiso 1 1 calc R
N21 N 0.2362(6) 0.7939(5) 0.5523(17) 0.072(4) Uani 1 1 d U
N22 N 0.2836(6) 0.7964(6) 0.452(2) 0.091(4) Uani 1 1 d U
H22 H 0.3217 0.7815 0.4685 0.110 Uiso 1 1 calc R
C23 C 0.2678(8) 0.8236(7) 0.326(3) 0.097(6) Uani 1 1 d U
H23 H 0.2938 0.8297 0.2445 0.116 Uiso 1 1 calc R
C24 C 0.2045(6) 0.8402(6) 0.344(2) 0.080(5) Uani 1 1 d U
H24 H 0.1775 0.8593 0.2758 0.096 Uiso 1 1 calc R
C25 C 0.1891(7) 0.8227(7) 0.484(2) 0.087(5) Uani 1 1 d U
H25 H 0.1490 0.8306 0.5262 0.104 Uiso 1 1 calc R
O1 O 0.3826(4) 0.8080(4) 1.0506(15) 0.084(3) Uani 1 1 d DU
H1A H 0.391(5) 0.781(5) 1.129(8) 0.101 Uiso 1 1 d D
H1B H 0.421(3) 0.802(5) 1.001(12) 0.101 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
C1 Nb C1 146.8(8) 15_566 12_767
C1 Nb C1 94.7(2) 15_566 .
C1 Nb C1 94.7(2) 12_767 .
C1 Nb C1 94.7(2) 15_566 6_564
C1 Nb C1 94.7(2) 12_767 6_564
C1 Nb C1 146.8(8) . 6_564
C1 Nb C2 71.9(6) 15_566 12_767
C1 Nb C2 141.3(6) 12_767 12_767
C1 Nb C2 76.7(5) . 12_767
C1 Nb C2 76.1(5) 6_564 12_767
C1 Nb C2 76.1(5) 15_566 6_564
C1 Nb C2 76.7(5) 12_767 6_564
C1 Nb C2 71.9(6) . 6_564
C1 Nb C2 141.3(6) 6_564 6_564
C2 Nb C2 132.6(6) 12_767 6_564
C1 Nb C2 76.7(5) 15_566 .
C1 Nb C2 76.1(5) 12_767 .
C1 Nb C2 141.3(6) . .
C1 Nb C2 71.9(6) 6_564 .
C2 Nb C2 132.6(6) 12_767 .
C2 Nb C2 69.4(10) 6_564 .
C1 Nb C2 141.3(6) 15_566 15_566
C1 Nb C2 71.9(6) 12_767 15_566
C1 Nb C2 76.1(5) . 15_566
C1 Nb C2 76.7(5) 6_564 15_566
C2 Nb C2 69.4(10) 12_767 15_566
C2 Nb C2 132.6(6) 6_564 15_566
C2 Nb C2 132.6(6) . 15_566
N1 Fe N1 180.0(5) . 13_566
N1 Fe N11 94.2(4) . .
N1 Fe N11 85.8(4) 13_566 .
N1 Fe N11 85.8(4) . 13_566
N1 Fe N11 94.2(4) 13_566 13_566
N11 Fe N11 180.0(7) . 13_566
N1 Fe N21 88.1(5) . .
N1 Fe N21 91.9(5) 13_566 .
N11 Fe N21 92.0(5) . .
N11 Fe N21 88.0(5) 13_566 .
N1 Fe N21 91.9(5) . 13_566
N1 Fe N21 88.1(5) 13_566 13_566
N11 Fe N21 88.0(5) . 13_566
N11 Fe N21 92.0(5) 13_566 13_566
N21 Fe N21 180.0(4) . 13_566
N1 C1 Nb 175.1(10) . .
C1 N1 Fe 160.1(11) . .
N2 C2 Nb 177.8(13) . .
C15 N11 N12 100.0(12) . .
C15 N11 Fe 134.5(11) . .
N12 N11 Fe 125.3(8) . .
C13 N12 N11 113.7(12) . .
N12 C13 C14 104.4(13) . .
C15 C14 C13 104.5(14) . .
N11 C15 C14 117.3(15) . .
C25 N21 N22 101.4(17) . .
C25 N21 Fe 137.1(13) . .
N22 N21 Fe 121.5(12) . .
C23 N22 N21 115.8(16) . .
N22 C23 C24 103.6(18) . .
C23 C24 C25 105.7(15) . .
N21 C25 C24 113.4(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb C1 2.216(13) 15_566
Nb C1 2.216(13) 12_767
Nb C1 2.216(13) .
Nb C1 2.216(13) 6_564
Nb C2 2.22(2) 12_767
Nb C2 2.22(2) 6_564
Nb C2 2.22(2) .
Nb C2 2.22(2) 15_566
Fe N1 2.026(10) .
Fe N1 2.026(10) 13_566
Fe N11 2.048(11) .
Fe N11 2.048(11) 13_566
Fe N21 2.057(15) .
Fe N21 2.057(15) 13_566
C1 N1 1.164(13) .
C2 N2 1.15(2) .
N11 C15 1.295(13) .
N11 N12 1.368(15) .
N12 C13 1.342(14) .
C13 C14 1.375(17) .
C14 C15 1.323(18) .
N21 C25 1.304(17) .
N21 N22 1.351(17) .
N22 C23 1.34(2) .
C23 C24 1.366(16) .
C24 C25 1.38(2) .
