Multimetastability in a Spin-Crossover Compound Leading to Different High-Spin-to-Low-Spin Relaxation Dynamics
Gavin A. Craig; Jose Sánchez Costa; Simon J. Teat; Olivier Roubeau; Dmitry S. Yufit; Judith A. K. Howard; Guillem Aromí; Inorganic Chemistry 52 (2013) 7203–7209; doi:10.1021/ic400776x

data_4335234
_publ_contact_author_name
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;
_publ_section_title
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 Multimetastability in a Spin-Crossover Compound Leading to Different
 High-Spin-to-Low-Spin Relaxation Dynamics
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7203
_journal_page_last               7209
_journal_paper_doi               10.1021/ic400776x
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C46 H34 Fe N10 O4, 2(Cl O4), H2 O, 2(C3 H6 O)'
_chemical_formula_sum            'C52 H48 Cl2 Fe N10 O15'
_chemical_formula_weight         1179.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-12-05
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:22:26, GUI svn.r4372)
;
_cell_angle_alpha                104.127(5)
_cell_angle_beta                 98.450(5)
_cell_angle_gamma                106.134(5)
_cell_formula_units_Z            2
_cell_length_a                   12.262(5)
_cell_length_b                   13.385(5)
_cell_length_c                   17.217(5)
_cell_measurement_reflns_used    5303
_cell_measurement_temperature    30
_cell_measurement_theta_max      29.794
_cell_measurement_theta_min      2.399
_cell_volume                     2561.5(16)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.049 (Bruker, 1999)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
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XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      30.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_unetI/netI     0.1286
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44241
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.60
_diffrn_reflns_theta_min         1.25
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           10.0
_diffrn_source_power             0.2
_diffrn_source_target            Mo
_diffrn_source_voltage           20.0
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.2090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.0605 before and 0.0462 after correction.
The Ratio of minimum to maximum transmission is 0.2252.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         14451
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0699
_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/[\s^2^(Fo^2^)+(0.0450P)^2^+3.2015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                8858
_reflns_number_total             14451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400776x_si_002.cif
_cod_data_source_block           jose2
_cod_database_code               4335234
_olex2_refinement_description
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1. others
 Fixed Uiso: H2(0.024) H1(0.02) H4(0.022) H1WA(0.024) H1WB(0.024) H10(0.013)
 H3(0.022) H5(0.012) H1A(0.011) H6(0.013) H13(0.014) H28(0.016) H19(0.015)
 H42(0.017) H45(0.017) H1SA(0.031) H1SB(0.031) H1SC(0.031) H5A(0.015)
 H27(0.018) H31(0.014) H8(0.014) H34(0.014) H25(0.017) H39(0.015) H43(0.018)
 H3A(0.016) H20(0.018) H44(0.018) H16(0.012) H22(0.016) H2A(0.015) H35(0.015)
 H12(0.015) H21(0.019) H6SA(0.03) H6SB(0.03) H6SC(0.03) H11(0.014) H36(0.015)
 H4SA(0.036) H4SB(0.036) H4SC(0.036) H4A(0.017) H26(0.018) H3SA(0.042)
 H3SB(0.042) H3SC(0.042) H3SD(0.064) H3SE(0.064) H3SF(0.064)
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