#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/42/4124213.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_4124213
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                   21.6751(19)
_cell_length_b                   21.6751(19)
_cell_length_c                   9.526(2)
_cell_measurement_pressure       300000
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      4.01
_cell_volume                     4475.4(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 0.474
_diffrn_measured_fraction_theta_max 0.474
_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  0.1235
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            9160
_diffrn_reflns_theta_full        27.15
_diffrn_reflns_theta_max         27.15
_diffrn_reflns_theta_min         4.01
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.641
_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    1.525
_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         1.462
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         1180
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0831
_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)+(0.2353P)²+19.9079P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2343
_refine_ls_wR_factor_ref         0.2714
_reflns_number_gt                877
_reflns_number_total             1180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b04303_si_005.cif
_cod_data_source_block           0.30_GPa
_cod_original_cell_volume        4475.6(13)
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               4124213
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 0.5596(3) 0.8678(3) 0.1964(12) 0.062(2) Uani 1 1 d DU
H1A H 0.547(5) 0.870(4) 0.103(3) 0.074 Uiso 1 1 d D
H1B H 0.559(4) 0.8282(18) 0.234(9) 0.074 Uiso 1 1 d D
C1 C 0.5142(3) 0.8474(3) 0.5527(13) 0.034(2) Uani 1 1 d U
C2 C 0.4406(3) 0.7593(3) 0.4308(14) 0.0342(17) Uani 1 1 d U
C13 C 0.6689(5) 1.0001(5) 0.2415(16) 0.066(4) Uani 1 1 d U
H13A H 0.6954 0.9804 0.1793 0.079 Uiso 1 1 calc R
C14 C 0.6779(5) 1.0547(5) 0.3077(18) 0.069(3) Uani 1 1 d U
H14A H 0.7120 1.0805 0.2978 0.082 Uiso 1 1 calc R
C15 C 0.6277(4) 1.0649(4) 0.3924(15) 0.056(3) Uani 1 1 d U
H15A H 0.6227 1.0994 0.4493 0.068 Uiso 1 1 calc R
C23 C 0.4277(5) 1.0178(5) 0.080(2) 0.074(4) Uani 1 1 d U
H23A H 0.4226 1.0430 0.0022 0.089 Uiso 1 1 calc R
C24 C 0.4124(5) 0.9584(5) 0.0884(17) 0.065(4) Uani 1 1 d U
H24A H 0.3948 0.9339 0.0188 0.079 Uiso 1 1 calc R
C25 C 0.4280(4) 0.9416(4) 0.2204(16) 0.055(3) Uani 1 1 d U
H25A H 0.4226 0.9021 0.2565 0.067 Uiso 1 1 calc R
Mn Mn 0.5000 1.0000 0.5000 0.0380(9) Uani 1 2 d SU
N1 N 0.5187(3) 0.8986(3) 0.5187(12) 0.047(3) Uani 1 1 d U
N2 N 0.4116(4) 0.7671(4) 0.3317(14) 0.059(3) Uani 1 1 d U
N11 N 0.5865(3) 1.0186(3) 0.3822(10) 0.047(3) Uani 1 1 d U
N12 N 0.6127(3) 0.9806(3) 0.2860(13) 0.056(3) Uani 1 1 d U
H12A H 0.5954 0.9474 0.2561 0.067 Uiso 1 1 calc R
N21 N 0.4520(3) 0.9885(3) 0.2924(12) 0.047(2) Uani 1 1 d U
N22 N 0.4514(4) 1.0347(3) 0.2018(15) 0.062(3) Uani 1 1 d U
H22A H 0.4648 1.0713 0.2198 0.074 Uiso 1 1 calc R
Nb Nb 0.5000 0.7500 0.6250 0.0270(8) 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 176.5(7) . .
N2 C2 Nb 176.5(7) . .
C14 C13 N12 104.9(10) . .
C13 C14 C15 107.4(9) . .
N11 C15 C14 111.3(10) . .
N22 C23 C24 108.4(14) . .
C23 C24 C25 104.6(12) . .
N21 C25 C24 111.8(9) . .
N11 Mn N11 180.0(3) . 9_676
N11 Mn N1 86.2(3) . 9_676
N11 Mn N1 93.8(3) 9_676 9_676
N11 Mn N1 93.8(3) . .
N11 Mn N1 86.2(3) 9_676 .
N1 Mn N1 180.000(1) 9_676 .
N11 Mn N21 91.9(3) . 9_676
N11 Mn N21 88.1(3) 9_676 9_676
N1 Mn N21 92.6(3) 9_676 9_676
N1 Mn N21 87.4(3) . 9_676
N11 Mn N21 88.1(3) . .
N11 Mn N21 91.9(3) 9_676 .
N1 Mn N21 87.4(3) 9_676 .
N1 Mn N21 92.6(3) . .
N21 Mn N21 180.000(2) 9_676 .
C1 N1 Mn 160.9(8) . .
C15 N11 N12 102.9(8) . .
C15 N11 Mn 131.2(7) . .
N12 N11 Mn 125.7(5) . .
C13 N12 N11 113.4(8) . .
N22 N21 C25 103.8(11) . .
N22 N21 Mn 119.6(6) . .
C25 N21 Mn 135.9(7) . .
C23 N22 N21 111.4(9) . .
C1 Nb C1 95.42(18) 15_566 6_564
C1 Nb C1 95.42(19) 15_566 .
C1 Nb C1 144.2(6) 6_564 .
C1 Nb C1 144.2(6) 15_566 12_767
C1 Nb C1 95.42(19) 6_564 12_767
C1 Nb C1 95.42(18) . 12_767
C1 Nb C2 75.1(3) 15_566 15_566
C1 Nb C2 143.1(4) 6_564 15_566
C1 Nb C2 72.7(4) . 15_566
C1 Nb C2 75.8(3) 12_767 15_566
C1 Nb C2 143.1(4) 15_566 .
C1 Nb C2 75.8(3) 6_564 .
C1 Nb C2 75.1(3) . .
C1 Nb C2 72.7(4) 12_767 .
C2 Nb C2 131.9(3) 15_566 .
C1 Nb C2 72.7(4) 15_566 6_564
C1 Nb C2 75.1(3) 6_564 6_564
C1 Nb C2 75.8(3) . 6_564
C1 Nb C2 143.1(4) 12_767 6_564
C2 Nb C2 131.9(3) 15_566 6_564
C2 Nb C2 70.3(5) . 6_564
C1 Nb C2 75.8(3) 15_566 12_767
C1 Nb C2 72.7(4) 6_564 12_767
C1 Nb C2 143.1(4) . 12_767
C1 Nb C2 75.1(3) 12_767 12_767
C2 Nb C2 70.3(5) 15_566 12_767
C2 Nb C2 131.9(3) . 12_767
C2 Nb C2 131.9(3) 6_564 12_767
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.162(11) .
C1 Nb 2.241(8) .
C2 N2 1.146(16) .
C2 Nb 2.263(11) .
C13 C14 1.355(16) .
C13 N12 1.357(13) .
C14 C15 1.374(16) .
C15 N11 1.347(11) .
C23 N22 1.32(2) .
C23 C24 1.332(14) .
C24 C25 1.352(19) .
C25 N21 1.332(13) .
Mn N11 2.221(8) .
Mn N11 2.221(8) 9_676
Mn N1 2.241(6) 9_676
Mn N1 2.241(6) .
Mn N21 2.248(10) 9_676
Mn N21 2.248(10) .
N11 N12 1.358(12) .
N21 N22 1.323(14) .
Nb C1 2.241(8) 15_566
Nb C1 2.241(8) 6_564
Nb C1 2.241(8) 12_767
Nb C2 2.263(12) 15_566
Nb C2 2.263(12) 6_564
Nb C2 2.263(12) 12_767
