#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/42/4124216.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_4124216
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 Mn2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Mn2 N24 Nb O4'
_chemical_formula_weight         1027.67
_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                   21.3237(18)
_cell_length_b                   21.3237(18)
_cell_length_c                   9.287(2)
_cell_measurement_pressure       1270000
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      4.08
_cell_volume                     4222.8(10)
_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 0.530
_diffrn_measured_fraction_theta_max 0.530
_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  0.0929
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            8932
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         4.08
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.634
_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            yellow
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.086
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1149
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.1048
_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)+(0.2340P)²+5.6000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2877
_refine_ls_wR_factor_ref         0.3217
_reflns_number_gt                874
_reflns_number_total             1149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b04303_si_005.cif
_cod_data_source_block           1.27_GPa
_cod_original_cell_volume        4223.0(12)
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               4124216
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
O1 O 0.5597(3) 0.8699(3) 0.1991(15) 0.058(3) Uani 1 1 d DU
H1A H 0.534(4) 0.851(5) 0.129(8) 0.070 Uiso 1 1 d D
H1B H 0.554(5) 0.854(5) 0.291(4) 0.070 Uiso 1 1 d D
C1 C 0.5172(4) 0.8486(4) 0.5537(16) 0.040(3) Uani 1 1 d U
C2 C 0.4406(4) 0.7610(4) 0.4264(16) 0.034(3) Uani 1 1 d U
C13 C 0.6730(5) 1.0038(5) 0.2487(17) 0.049(3) Uani 1 1 d U
H13A H 0.7008 0.9838 0.1867 0.059 Uiso 1 1 calc R
C14 C 0.6814(5) 1.0589(5) 0.316(2) 0.065(4) Uani 1 1 d U
H14A H 0.7165 1.0847 0.3100 0.078 Uiso 1 1 calc R
C15 C 0.6280(5) 1.0699(4) 0.3978(17) 0.053(3) Uani 1 1 d U
H15A H 0.6213 1.1046 0.4562 0.063 Uiso 1 1 calc R
C23 C 0.4258(6) 1.0180(6) 0.072(2) 0.076(4) Uani 1 1 d U
H23A H 0.4196 1.0444 -0.0063 0.091 Uiso 1 1 calc R
C24 C 0.4094(5) 0.9562(5) 0.078(2) 0.061(4) Uani 1 1 d U
H24A H 0.3918 0.9312 0.0068 0.073 Uiso 1 1 calc R
C25 C 0.4252(5) 0.9400(4) 0.2167(18) 0.050(3) Uani 1 1 d U
H25A H 0.4183 0.9005 0.2561 0.060 Uiso 1 1 calc R
Mn Mn 0.5000 1.0000 0.5000 0.0401(11) Uani 1 2 d SU
N1 N 0.5232(4) 0.8997(3) 0.5162(14) 0.050(3) Uani 1 1 d U
N2 N 0.4111(4) 0.7678(4) 0.3242(17) 0.060(3) Uani 1 1 d U
N11 N 0.5873(3) 1.0225(3) 0.3790(11) 0.042(3) Uani 1 1 d U
N12 N 0.6150(4) 0.9834(3) 0.2903(15) 0.051(3) Uani 1 1 d U
H12A H 0.5985 0.9488 0.2615 0.062 Uiso 1 1 calc R
N21 N 0.4513(3) 0.9870(3) 0.2876(14) 0.045(3) Uani 1 1 d U
N22 N 0.4515(5) 1.0341(3) 0.1936(17) 0.059(3) Uani 1 1 d U
H22A H 0.4667 1.0706 0.2110 0.071 Uiso 1 1 calc R
Nb Nb 0.5000 0.7500 0.6250 0.0294(10) Uani 1 4 d SU
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'
Mn Mn 0.3368 0.7283 '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
N1 C1 Nb 176.9(7) . .
N2 C2 Nb 178.4(9) . .
C14 C13 N12 105.5(11) . .
C13 C14 C15 107.0(10) . .
N11 C15 C14 109.4(11) . .
N22 C23 C24 109.0(15) . .
C23 C24 C25 102.6(13) . .
N21 C25 C24 112.4(9) . .
N1 Mn N1 180.000(1) . 9_676
N1 Mn N11 86.8(3) . 9_676
N1 Mn N11 93.2(3) 9_676 9_676
N1 Mn N11 93.2(3) . .
N1 Mn N11 86.8(3) 9_676 .
N11 Mn N11 180.0(4) 9_676 .
N1 Mn N21 92.5(4) . .
N1 Mn N21 87.5(4) 9_676 .
N11 Mn N21 91.7(3) 9_676 .
N11 Mn N21 88.3(3) . .
N1 Mn N21 87.5(4) . 9_676
N1 Mn N21 92.5(4) 9_676 9_676
N11 Mn N21 88.3(3) 9_676 9_676
N11 Mn N21 91.7(3) . 9_676
N21 Mn N21 180.000(3) . 9_676
C1 N1 Mn 156.3(9) . .
N12 N11 C15 105.6(8) . .
N12 N11 Mn 123.8(6) . .
C15 N11 Mn 129.5(8) . .
N11 N12 C13 112.5(8) . .
C25 N21 N22 104.2(12) . .
C25 N21 Mn 136.6(8) . .
N22 N21 Mn 118.8(7) . .
C23 N22 N21 111.7(10) . .
C1 Nb C1 95.0(2) 12_767 6_564
C1 Nb C1 95.0(2) 12_767 .
C1 Nb C1 145.5(7) 6_564 .
C1 Nb C1 145.5(7) 12_767 15_566
C1 Nb C1 95.0(2) 6_564 15_566
C1 Nb C1 95.0(2) . 15_566
C1 Nb C2 76.3(4) 12_767 15_566
C1 Nb C2 142.2(5) 6_564 15_566
C1 Nb C2 72.3(5) . 15_566
C1 Nb C2 75.6(4) 15_566 15_566
C1 Nb C2 75.6(4) 12_767 12_767
C1 Nb C2 72.3(5) 6_564 12_767
C1 Nb C2 142.2(5) . 12_767
C1 Nb C2 76.3(4) 15_566 12_767
C2 Nb C2 69.9(5) 15_566 12_767
C1 Nb C2 72.3(5) 12_767 .
C1 Nb C2 76.3(4) 6_564 .
C1 Nb C2 75.6(4) . .
C1 Nb C2 142.2(5) 15_566 .
C2 Nb C2 132.2(3) 15_566 .
C2 Nb C2 132.2(3) 12_767 .
C1 Nb C2 142.2(5) 12_767 6_564
C1 Nb C2 75.6(4) 6_564 6_564
C1 Nb C2 76.3(4) . 6_564
C1 Nb C2 72.3(5) 15_566 6_564
C2 Nb C2 132.2(3) 15_566 6_564
C2 Nb C2 132.2(3) 12_767 6_564
C2 Nb C2 69.9(5) . 6_564
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.151(12) .
C1 Nb 2.234(9) .
C2 N2 1.148(17) .
C2 Nb 2.250(13) .
C13 C14 1.344(17) .
C13 N12 1.367(13) .
C14 C15 1.388(18) .
C15 N11 1.342(12) .
C23 N22 1.30(2) .
C23 C24 1.366(16) .
C24 C25 1.37(2) .
C25 N21 1.321(14) .
Mn N1 2.201(8) .
Mn N1 2.201(8) 9_676
Mn N11 2.227(8) 9_676
Mn N11 2.227(8) .
Mn N21 2.247(12) .
Mn N21 2.247(12) 9_676
N11 N12 1.312(13) .
N21 N22 1.331(16) .
Nb C1 2.234(9) 12_767
Nb C1 2.234(9) 6_564
Nb C1 2.234(9) 15_566
Nb C2 2.250(13) 15_566
Nb C2 2.250(13) 12_767
Nb C2 2.250(13) 6_564
