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_7704305
_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 Pd2'
_chemical_formula_sum            'C56 H40 Fe2 N16 Pd2'
_chemical_formula_weight         1261.54
_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     direct
_audit_creation_date             2020-04-27
_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                   14.6772(11)
_cell_length_b                   7.1611(4)
_cell_length_c                   28.221(2)
_cell_measurement_reflns_used    3284
_cell_measurement_temperature    84.9(10)
_cell_measurement_theta_max      29.7210
_cell_measurement_theta_min      4.0030
_cell_volume                     2966.2(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      N~2~
_diffrn_ambient_temperature      84.9(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.928
_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    -61.00 -36.00   0.50   25.00    --    0.10 -29.00 -25.00   50
  2  \w     26.00  51.00   0.50   25.00    --    0.10  29.00 135.00   50
  3  \w      6.00  31.00   0.50   25.00    --    0.10 -82.00 -60.00   50
  4  \w    -76.00  -4.00   0.50   25.00    --    0.10 -77.00-120.00  144
  5  \w     -8.00  20.00   0.50   25.00    --    0.10 -82.00   0.00   56
  6  \w    -51.00 -26.00   0.50   25.00    --    0.10 -82.00 -60.00   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      -0.0103347000
_diffrn_orient_matrix_UB_12      0.0949808000
_diffrn_orient_matrix_UB_13      -0.0047031000
_diffrn_orient_matrix_UB_21      -0.0149694000
_diffrn_orient_matrix_UB_22      0.0114745000
_diffrn_orient_matrix_UB_23      0.0237106000
_diffrn_orient_matrix_UB_31      0.0447582000
_diffrn_orient_matrix_UB_32      0.0257646000
_diffrn_orient_matrix_UB_33      0.0068769000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            11530
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.650
_diffrn_reflns_theta_min         3.479
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60336
_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 reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_platon_squeeze_details          TITL
_refine_diff_density_max         1.919
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         2166
_refine_ls_number_restraints     861
_refine_ls_restrained_S_all      1.815
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0339P)^2^+43.9337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1813
_reflns_number_total             2166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00866d2.cif
_cod_data_source_block           compound1_85K
_cod_depositor_comments
'Adding full bibliography for 7704300--7704305.cif.'
_cod_database_code               7704305
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.849
_reflns_odcompleteness_completeness 99.43
_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
 N1A-C1A = C5A-C3A = C2A-C4A
 1.38 with sigma of 0.02
 Fe1-N1A
 2.016 with sigma of 0.02
 Fe1-N1B
 2.017 with sigma of 0.02
 N1B-C5B = C4B-C3B = C2B-C1B
 1.38 with sigma of 0.02
 C3B-C6B
 1.5 with sigma of 0.02
 C7B-C8B
 1.5 with sigma of 0.02
 C8B-C9B = C10B-C11B = C12B-N2B
 1.38 with sigma of 0.02
 C9A-C6A
 3 with sigma of 0.02
 C9B-C6B
 3 with sigma of 0.02
 C6A-C7A
 1.38 with sigma of 0.02
 C6B-C7B
 1.38 with sigma of 0.02
3. Restrained planarity
 N1B, N2B, C1B, C2B, C3B, C4B, C5B, 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
N1A \\sim N1B \\sim N2A \\sim N2B \\sim C1A \\sim C1B \\sim C2A \\sim C2B \\sim
C3A \\sim C3B \\sim C4A \\sim C4B \\sim C5A \\sim C5B \\sim C6A \\sim C6B \\sim
C7A \\sim C7B \\sim C8A \\sim C8B \\sim C9A \\sim C9B \\sim C10A \\sim C10B
\\sim C11A \\sim C11B \\sim C12A \\sim C12B: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(N1A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C3A)
\\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C1A) \\sim Ueq, 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(C6A) \\sim Ueq, Uanis(C6B) \\sim Ueq,
Uanis(C7A) \\sim Ueq, Uanis(C7B) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C9A)
\\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C12A) \\sim Ueq,
Uanis(N2A) \\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:
with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 N1A, N1B, N2A, N2B, C1A, C1B, C2A, C2B, C3A, C3B, C4A, C4B, C5A, C5B, C6A,
 C6B, C7A, C7B, C8A, C8B, C9A, C9B, C10A, C10B, C11A, C11B, C12A, C12B
 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) C5A(0.25) H5A(0.25) C4A(0.25) H4A(0.25) C3A(0.25)
 C2A(0.25) H2A(0.25) C1A(0.25) H1A(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) C9A(0.25) H9A(0.25) C10A(0.25) H10A(0.25) C11A(0.25)
 H11A(0.25) C12A(0.25) H12A(0.25) N2A(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:
 C5A(H5A), C4A(H4A), C2A(H2A), C1A(H1A), C5B(H5B), C4B(H4B), C2B(H2B),
 C1B(H1B), C6A(H6A), C6B(H6B), C7A(H7A), C7B(H7B), C9A(H9A), C10A(H10A),
 C11A(H11A), C12A(H12A), C9B(H9B), C10B(H10B), C11B(H11B), C12B(H12B)
7.b Fitted hexagon refined as free rotating group:
 N1A(C5A,C4A,C3A,C2A,C1A), N1B(C5B,C4B,C3B,C2B,C1B), C8A(C9A,C10A,C11A,C12A,
 N2A), C8B(C9B,C10B,C11B,C12B,N2B)
;
_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 1.739
_oxdiff_exptl_absorpt_empirical_full_min 0.720