Temperature-dependent hysteretic two-step spin crossover in two-dimensional Hofmann-type compounds.
Li, Yue; Liu, Min; Yao, Zi-Shuo; Tao, Jun; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7245–7251; doi:10.1039/d0dt00866d

data_7704303
_publ_section_title
;
 Temperature-dependent hysteretic two-step spin crossover in
 two-dimensional Hofmann-type compounds.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7245
_journal_page_last               7251
_journal_paper_doi               10.1039/d0dt00866d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C56 H40 Fe2 N16 Pt2'
_chemical_formula_sum            'C56 H40 Fe2 N16 Pt2'
_chemical_formula_weight         1438.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-29 deposited with the CCDC.	2020-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.4043(4)
_cell_length_b                   15.1012(6)
_cell_length_c                   28.6158(14)
_cell_measurement_reflns_used    4480
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      29.7690
_cell_measurement_theta_min      4.1050
_cell_volume                     3199.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298(1)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -46.00 -18.00   0.50   25.00    --    0.00 -63.00 101.00   56
  2  \w    -56.00 -31.00   0.50   25.00    --    0.00 -70.00-120.00   50
  3  \w    -63.00  24.00   0.50   25.00    --    0.00 -82.00-150.00  174
  4  \w    -63.00 -13.00   0.50   25.00    --    0.00 -82.00  30.00  100
  5  \w    -46.00 -21.00   0.50   25.00    --    0.00 -38.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0254066000
_diffrn_orient_matrix_UB_12      0.0204792000
_diffrn_orient_matrix_UB_13      -0.0149118000
_diffrn_orient_matrix_UB_21      0.0274181000
_diffrn_orient_matrix_UB_22      0.0124609000
_diffrn_orient_matrix_UB_23      0.0612039000
_diffrn_orient_matrix_UB_31      0.0284420000
_diffrn_orient_matrix_UB_32      0.0063002000
_diffrn_orient_matrix_UB_33      -0.0721825000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            10978
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.636
_diffrn_reflns_theta_min         3.483
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.848
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
TITL rt_942    I m m a      R = 0.07
CELL    7.4043   15.1012   28.6158     90.00     90.00     90.00
SPGR Imma
C101 0.500 0.756 0.203 !      14.19 eA-3
C102 0.250 0.750 0.250 !      11.03 eA-3
Q103 0.500 0.252 0.477 !       2.87 eA-3
C104 1.000 0.746 0.211 !       2.83 eA-3
C105 0.781 0.252 0.203 !       2.77 eA-3
Q106 0.934 0.750 0.031 !       2.27 eA-3
C107 0.500 0.748 0.250 !       2.21 eA-3
Q108 0.908 0.776 0.008 !       2.16 eA-3
C109 0.195 0.755 0.133 !       2.06 eA-3
C110 0.366 0.250 0.289 !       1.93 eA-3
Q111 1.000 0.752 0.016 !       1.80 eA-3
C112 0.239 0.756 0.203 !       1.62 eA-3
Q113 1.000 0.255 0.219 !       1.54 eA-3
Q114 1.000 0.015 0.202 !       1.53 eA-3
C115 0.196 0.748 0.180 !       1.51 eA-3
Q116 0.120 0.243 0.031 !       1.40 eA-3
Q117 0.500 0.441 0.219 !       1.40 eA-3
C118 0.720 0.755 0.172 !       1.39 eA-3
C119 0.307 0.751 0.125 !       1.24 eA-3
Q120 1.000 0.940 0.384 !       1.23 eA-3
Q121 1.000 0.609 0.170 !       1.21 eA-3
C122 0.250 0.219 0.256 !       1.17 eA-3
C123 0.500 0.756 0.156 !       1.12 eA-3
Q124 0.567 0.685 0.211 !       1.10 eA-3
C125 0.740 0.745 0.391 !       1.05 eA-3
Q126 0.500 0.126 0.140 !       1.04 eA-3
Q127 0.500 0.218 0.294 !       1.02 eA-3
Q128 0.575 0.251 0.188 !       1.01 eA-3
Q129 0.253 0.058 0.004 !       1.01 eA-3
Q130 1.000 0.749 0.055 !       0.97 eA-3
C131 0.500 0.750 0.117 !       0.96 eA-3
Q132 0.500 0.450 0.189 !       0.95 eA-3
Q133 0.500 0.626 0.248 !       0.94 eA-3
Q134 1.000 0.813 0.030 !       0.93 eA-3
Q135 0.810 0.656 0.298 !       0.93 eA-3
Q136 0.500 0.660 0.085 !       0.93 eA-3
C137 0.197 0.706 0.223 !       0.93 eA-3
Q138 1.000 0.342 0.186 !       0.92 eA-3
Q139 1.000 0.894 0.363 !       0.91 eA-3
Q140 0.500 0.394 0.863 !       0.91 eA-3
C141 0.776 0.811 0.269 !       0.90 eA-3
Q142 0.555 0.126 0.384 !       0.90 eA-3
Q143 0.563 0.723 0.133 !       0.90 eA-3
Q144 0.790 1.000 0.000 !       0.89 eA-3
C145 0.739 0.250 0.102 !       0.88 eA-3
Q146 1.000 0.753 0.156 !       0.88 eA-3
Q147 0.500 0.059 0.249 !       0.87 eA-3
Q148 0.223 0.311 0.007 !       0.86 eA-3
Q149 0.185 0.660 0.109 !       0.86 eA-3
Q150 0.782 0.743 0.047 !       0.85 eA-3
Q151 0.500 0.789 0.007 !       0.85 eA-3
Q152 0.500 0.502 0.022 !       0.84 eA-3
Q153 0.558 0.128 0.099 !       0.84 eA-3
Q154 0.751 0.874 0.094 !       0.83 eA-3
Q155 0.500 0.616 0.092 !       0.83 eA-3
C156 0.598 0.284 0.253 !       0.82 eA-3
C157 1.000 0.749 0.117 !       0.82 eA-3
Q158 0.194 0.683 0.151 !       0.82 eA-3
Q159 0.500 0.756 0.406 !       0.81 eA-3
Q160 0.745 0.801 0.057 !       0.81 eA-3
Q161 0.747 0.185 0.191 !       0.81 eA-3
Q162 1.000 0.248 0.055 !       0.81 eA-3
Q163 0.750 0.531 0.248 !       0.81 eA-3
Q164 0.246 0.251 0.031 !       0.80 eA-3
Q165 1.000 0.644 0.273 !       0.79 eA-3
Q166 0.063 0.254 0.492 !       0.79 eA-3
Q167 0.249 0.686 0.191 !       0.78 eA-3
Q168 0.500 0.563 0.241 !       0.78 eA-3
Q169 0.500 0.157 0.180 !       0.78 eA-3
Q170 1.000 0.937 0.154 !       0.78 eA-3
Q171 0.686 0.249 0.367 !       0.78 eA-3
Q172 0.500 0.356 0.403 !       0.78 eA-3
Q173 0.621 0.850 0.134 !       0.77 eA-3
Q174 0.500 0.125 0.344 !       0.75 eA-3
Q175 0.500 0.455 0.102 !       0.75 eA-3
C176 0.500 0.251 0.250 !       0.75 eA-3
Q177 0.804 0.370 0.004 !       0.75 eA-3
C178 1.000 0.792 0.264 !       0.74 eA-3
Q179 0.932 0.182 0.023 !       0.74 eA-3
Q180 0.500 0.088 0.004 !       0.73 eA-3
C181 0.772 0.250 0.328 !       0.73 eA-3
Q182 0.500 0.657 0.310 !       0.73 eA-3
Q183 0.130 0.246 0.070 !       0.72 eA-3
Q184 0.229 0.675 0.492 !       0.72 eA-3
Q185 0.628 0.189 0.000 !       0.72 eA-3
Q186 1.000 0.275 0.086 !       0.70 eA-3
Q187 0.300 0.744 0.008 !       0.70 eA-3
Q188 1.000 0.505 0.246 !       0.69 eA-3
Q189 0.864 0.544 0.014 !       0.67 eA-3
Q190 0.315 0.662 0.074 !       0.67 eA-3
Q191 1.000 0.157 0.217 !       0.66 eA-3
Q192 1.000 0.323 0.134 !       0.66 eA-3
Q193 1.000 0.449 0.062 !       0.65 eA-3
Q194 1.000 0.281 0.296 !       0.64 eA-3
Q195 0.815 0.104 0.125 !       0.64 eA-3
Q196 0.500 0.972 0.220 !       0.64 eA-3
Q197 0.935 0.309 0.208 !       0.64 eA-3
Q198 0.934 0.161 0.251 !       0.64 eA-3
Q199 0.066 0.839 0.749 !       0.64 eA-3
;
_refine_diff_density_max         2.371
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         2310
_refine_ls_number_restraints     211
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0479P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1996
_reflns_number_total             2310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00866d2.cif
_cod_data_source_block           compound2_298K
_cod_depositor_comments
'Adding full bibliography for 7704300--7704305.cif.'
_cod_database_code               7704303
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 98.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7B-C8B
 1.5 with sigma of 0.02
 N2B-C8B = C9B-C10B = C11B-C12B
 1.38 with sigma of 0.02
 Fe1-N1A
 2.207 with sigma of 0.02
 N1A-C1A = C2A-C3A = C4A-C5A
 1.38 with sigma of 0.02
 Fe1-N1B
 2.207 with sigma of 0.02
 N1B-C1B = C2B-C3B = C4B-C5B
 1.38 with sigma of 0.02
 C3A-C6A
 1.5 with sigma of 0.02
 C3B-C6B
 1.5 with sigma of 0.02
 C6B-C7B
 1.38 with sigma of 0.02
 C8A-C9A = C10A-C11A = C12A-N2A
 1.38 with sigma of 0.02
 C8A-C7A
 1.5 with sigma of 0.02
 N2A-C7A
 2.363 with sigma of 0.02
 C9A-C6A
 3.1 with sigma of 0.02
 C6A-C7A
 1.38 with sigma of 0.02
3. Restrained planarity
 N1A, N2B, C2A, C3A, C4A, C5A, C6B, C7B, C8B, C9B, C10B, C11B, C12B
 with sigma of 0.1
 N1A, N2A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A, C12A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(N1B) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C2B) \\sim Ueq, Uanis(C3B)
\\sim Ueq, Uanis(C4B) \\sim Ueq, Uanis(C5B) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N1B) \\sim Ueq, Uanis(C5B) \\sim Ueq, Uanis(C4B) \\sim Ueq, Uanis(C3B)
\\sim Ueq, Uanis(C2B) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(N1A) \\sim Ueq,
Uanis(C1A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A)
\\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C7B) \\sim Ueq, Uanis(C6B) \\sim Ueq,
Uanis(C8B) \\sim Ueq, Uanis(C9B) \\sim Ueq, Uanis(C10B) \\sim Ueq, Uanis(C11B)
\\sim Ueq, Uanis(C12B) \\sim Ueq, Uanis(N2B) \\sim Ueq, Uanis(C6A) \\sim Ueq,
Uanis(C7A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C12A)
\\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C9A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: N1A(0.25) C1A(0.25) H1A(0.25) C2A(0.25) H2A(0.25) C3A(0.25)
 C4A(0.25) H4A(0.25) C5A(0.25) H5A(0.25) N1B(0.25) C5B(0.25) H5B(0.25)
 C4B(0.25) H4B(0.25) C3B(0.25) C2B(0.25) H2B(0.25) C1B(0.25) H1B(0.25)
 C6A(0.25) H6A(0.25) C6B(0.25) H6B(0.25) C7A(0.25) H7A(0.25) C7B(0.25)
 H7B(0.25) C8A(0.25) N2A(0.25) C12A(0.25) H12A(0.25) C11A(0.25) H11A(0.25)
 C10A(0.25) H10A(0.25) C9A(0.25) H9A(0.25) C8B(0.25) C9B(0.25) H9B(0.25)
 C10B(0.25) H10B(0.25) C11B(0.25) H11B(0.25) C12B(0.25) H12B(0.25) N2B(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C4A(H4A), C5A(H5A), C5B(H5B), C4B(H4B), C2B(H2B),
 C1B(H1B), C6A(H6A), C6B(H6B), C7A(H7A), C7B(H7B), C12A(H12A), C11A(H11A),
 C10A(H10A), C9A(H9A), C9B(H9B), C10B(H10B), C11B(H11B), C12B(H12B)
7.b Fitted hexagon refined as free rotating group:
 N1A(C1A,C2A,C3A,C4A,C5A), N1B(C5B,C4B,C3B,C2B,C1B), C8A(N2A,C12A,C11A,C10A,
 C9A), C8B(C9B,C10B,C11B,C12B,N2B)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 16.870
_oxdiff_exptl_absorpt_empirical_full_min 0.283