#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/42/4124221.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_4124221
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                   21.140(3)
_cell_length_b                   21.140(3)
_cell_length_c                   8.903(2)
_cell_measurement_pressure       2710000
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.16
_cell_measurement_theta_min      5.46
_cell_volume                     3978.7(12)
_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 0.413
_diffrn_measured_fraction_theta_max 0.413
_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  0.1581
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            6506
_diffrn_reflns_theta_full        26.16
_diffrn_reflns_theta_max         26.16
_diffrn_reflns_theta_min         5.46
_exptl_absorpt_coefficient_mu    0.982
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.682
_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            red
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         822
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.1129
_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)+(0.2400P)²+20.3000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3092
_refine_ls_wR_factor_ref         0.3485
_reflns_number_gt                609
_reflns_number_total             822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b04303_si_005.cif
_cod_data_source_block           2.71_GPa
_cod_original_cell_volume        3978.5(13)
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               4124221
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 0.039(2) Uani 1 4 d SU
Mn2 Mn 0.5000 1.0000 0.5000 0.051(3) Uani 1 2 d SU
N21 N 0.5445(6) 0.9848(6) 0.284(3) 0.069(7) Uani 1 1 d U
C2 C 0.5562(8) 0.7635(7) 0.400(4) 0.057(5) Uani 1 1 d U
N1 N 0.4749(7) 0.9002(6) 0.520(4) 0.076(7) Uani 1 1 d U
N22 N 0.5509(10) 1.0318(8) 0.184(4) 0.105(9) Uani 1 1 d DU
H22A H 0.5406 1.0701 0.2055 0.126 Uiso 1 1 calc R
N11 N 0.5881(9) 0.9762(7) 0.614(3) 0.083(8) Uani 1 1 d U
C13 C 0.6713(10) 0.9912(10) 0.734(5) 0.090(9) Uani 1 1 d U
H13A H 0.6988 1.0108 0.8014 0.107 Uiso 1 1 calc R
C1 C 0.4815(8) 0.8481(8) 0.552(5) 0.072(8) Uani 1 1 d U
C15 C 0.6303(9) 0.9281(10) 0.596(5) 0.082(8) Uani 1 1 d U
H15A H 0.6213 0.8924 0.5390 0.098 Uiso 1 1 calc R
C23 C 0.5750(16) 1.0157(17) 0.042(4) 0.150(14) Uani 1 1 d DU
H23A H 0.5826 1.0424 -0.0387 0.180 Uiso 1 1 calc R
C24 C 0.5848(11) 0.9527(12) 0.051(6) 0.104(10) Uani 1 1 d U
H24A H 0.5950 0.9252 -0.0272 0.125 Uiso 1 1 calc R
N2 N 0.5892(8) 0.7734(10) 0.334(4) 0.097(8) Uani 1 1 d U
C14 C 0.6830(10) 0.9356(10) 0.664(4) 0.085(9) Uani 1 1 d U
H14A H 0.7190 0.9102 0.6646 0.102 Uiso 1 1 calc R
C25 C 0.5758(9) 0.9374(8) 0.206(5) 0.077(9) Uani 1 1 d U
H25A H 0.5895 0.8999 0.2502 0.093 Uiso 1 1 calc R
N12 N 0.6173(9) 1.0129(10) 0.696(5) 0.096(8) Uani 1 1 d U
H12A H 0.6030 1.0491 0.7239 0.115 Uiso 1 1 calc R
O1 O 0.6243(10) 0.8145(8) 1.043(4) 0.121(8) Uani 1 1 d DU
H1A H 0.603(7) 0.789(10) 0.974(12) 0.145 Uiso 1 1 d D
H1B H 0.615(13) 0.806(12) 1.144(5) 0.145 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'
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
C1 Nb1 C1 95.0(6) 12_767 6_564
C1 Nb1 C1 146(2) 12_767 15_566
C1 Nb1 C1 95.0(6) 6_564 15_566
C1 Nb1 C1 95.0(6) 12_767 .
C1 Nb1 C1 146(2) 6_564 .
C1 Nb1 C1 95.0(6) 15_566 .
C1 Nb1 C2 75.8(11) 12_767 6_564
C1 Nb1 C2 73.9(10) 6_564 6_564
C1 Nb1 C2 138.6(12) 15_566 6_564
C1 Nb1 C2 76.8(10) . 6_564
C1 Nb1 C2 73.9(10) 12_767 12_767
C1 Nb1 C2 138.6(12) 6_564 12_767
C1 Nb1 C2 76.8(10) 15_566 12_767
C1 Nb1 C2 75.8(11) . 12_767
C2 Nb1 C2 136.7(7) 6_564 12_767
C1 Nb1 C2 76.8(10) 12_767 15_566
C1 Nb1 C2 75.8(11) 6_564 15_566
C1 Nb1 C2 73.9(10) 15_566 15_566
C1 Nb1 C2 138.6(12) . 15_566
C2 Nb1 C2 136.7(7) 6_564 15_566
C2 Nb1 C2 62.9(11) 12_767 15_566
C1 Nb1 C2 138.6(12) 12_767 .
C1 Nb1 C2 76.8(10) 6_564 .
C1 Nb1 C2 75.8(11) 15_566 .
C1 Nb1 C2 73.9(10) . .
C2 Nb1 C2 62.9(11) 6_564 .
C2 Nb1 C2 136.7(7) 12_767 .
C2 Nb1 C2 136.7(7) 15_566 .
N21 Mn2 N21 180.000(7) 9_676 .
N21 Mn2 N11 90.4(9) 9_676 9_676
N21 Mn2 N11 89.6(9) . 9_676
N21 Mn2 N11 89.6(9) 9_676 .
N21 Mn2 N11 90.4(9) . .
N11 Mn2 N11 180.000(4) 9_676 .
N21 Mn2 N1 92.0(9) 9_676 9_676
N21 Mn2 N1 88.0(9) . 9_676
N11 Mn2 N1 86.9(6) 9_676 9_676
N11 Mn2 N1 93.1(7) . 9_676
N21 Mn2 N1 88.0(9) 9_676 .
N21 Mn2 N1 92.0(9) . .
N11 Mn2 N1 93.1(7) 9_676 .
N11 Mn2 N1 86.9(6) . .
N1 Mn2 N1 180.000(2) 9_676 .
N22 N21 C25 99(3) . .
N22 N21 Mn2 121.6(17) . .
C25 N21 Mn2 139.4(18) . .
N2 C2 Nb1 160(3) . .
C1 N1 Mn2 157.0(17) . .
N21 N22 C23 117(2) . .
N12 N11 C15 102(2) . .
N12 N11 Mn2 124.0(14) . .
C15 N11 Mn2 133(2) . .
N12 C13 C14 111(3) . .
N12 C13 C15 72(2) . .
C14 C13 C15 38.8(14) . .
N1 C1 Nb1 175(2) . .
C14 C15 N11 115(3) . .
C14 C15 C13 41.7(15) . .
N11 C15 C13 73.6(17) . .
C24 C23 N22 104(3) . .
C23 C24 C25 105(4) . .
C15 C14 C13 99(2) . .
N21 C25 C24 112.5(19) . .
N11 N12 C13 112(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 C1 2.21(2) 12_767
Nb1 C1 2.21(2) 6_564
Nb1 C1 2.21(2) 15_566
Nb1 C1 2.21(2) .
Nb1 C2 2.34(3) 6_564
Nb1 C2 2.34(3) 12_767
Nb1 C2 2.34(3) 15_566
Nb1 C2 2.34(3) .
Mn2 N21 2.16(3) 9_676
Mn2 N21 2.16(3) .
Mn2 N11 2.18(2) 9_676
Mn2 N11 2.18(2) .
Mn2 N1 2.183(14) 9_676
Mn2 N1 2.183(13) .
N21 N22 1.34(4) .
N21 C25 1.39(3) .
C2 N2 0.94(3) .
N1 C1 1.14(2) .
N22 C23 1.400(3) .
N11 N12 1.23(4) .
N11 C15 1.36(3) .
C13 N12 1.28(3) .
C13 C14 1.36(4) .
C13 C15 2.01(5) .
C15 C14 1.28(3) .
C23 C24 1.35(4) .
C24 C25 1.44(6) .
