Guest water-induced structural transformation and spin-crossover variation of a two-dimensional Hofmann-type compound.
Liu, Zhi-Kun; Sun, Ke; Xue, Jin-Peng; Yao, Zi-Shuo; Tao, Jun; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7522–7526; doi:10.1039/d4dt00435c

data_7715622
_publ_section_title
;
 Guest water-induced structural transformation and spin-crossover
 variation of a two-dimensional Hofmann-type compound.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7522
_journal_page_last               7526
_journal_paper_doi               10.1039/d4dt00435c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C22 H14 Fe N14 O4 Pt'
_chemical_formula_sum            'C22 H14 Fe N14 O4 Pt'
_chemical_formula_weight         789.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-03-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2024-03-16 deposited with the CCDC.	2024-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.248(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.0552(11)
_cell_length_b                   7.0129(2)
_cell_length_c                   14.6062(5)
_cell_measurement_reflns_used    5048
_cell_measurement_temperature    180
_cell_measurement_theta_max      29.8170
_cell_measurement_theta_min      3.7630
_cell_volume                     2634.19(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      180.00
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -63.00  31.00   0.25    8.66    --    0.10 -82.00-180.00  376
  2  \w      3.00  30.00   0.25    8.66    --    0.10  38.00  60.00  108
  3  \w    -49.00 -22.00   0.25    8.66    --    0.10 -82.00 -60.00  108
  4  \w      7.00  80.00   0.25    8.66    --    0.10  38.00-150.00  292
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9199
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         3.874
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.702
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         2520
_refine_ls_number_restraints     1593
_refine_ls_restrained_S_all      0.822
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+19.2124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1973
_reflns_number_total             2520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00435c2.cif
_cod_data_source_block           180k-dry-c2
_cod_depositor_comments
'Adding full bibliography for 7715619--7715624.cif.'
_cod_database_code               7715622
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.384
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained planarity
 N2, N5B, N3A, N3B, N6B, N6A, N4A, N4B, N5A, C2A, C2B, C3A, C3B, C4A, C4B, C5A,
  C6A, C7A, C8A, C9A, C10A, C5B, C6B, C7B, C8B, C9B, C10B
 with sigma of 0.1
 N10A, N12A, N9A, N11A, N8, N9B, N10B, N11B, N12B, C18A, C13B, C18B, C16A,
 C12B, C20B, C16B, C20A, C14B, C12A, C13A, C14A, C19B, C17B, C15B, C19A, C15A,
 C17A
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O3B)=Sof(O2B)=Sof(O4B)=Sof(O1B)=Sof(N5B)=Sof(N3B)=Sof(N6B)=Sof(N9B)=
 Sof(N4B)=Sof(N10B)=Sof(N11B)=Sof(N12B)=Sof(C13B)=Sof(H13B)=Sof(C2B)=Sof(H2B)=
 Sof(C3B)=Sof(H3B)=Sof(C12B)=Sof(H12B)=Sof(C20B)=Sof(H20B)=Sof(C19B)=Sof(H19B)=
 Sof(C18B)=Sof(H18B)=Sof(C17B)=Sof(H17B)=Sof(C16B)=Sof(C15B)=Sof(C4B)=Sof(H4B)=
 Sof(C14B)=Sof(H14B)=Sof(C5B)=Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=
 Sof(H8B)=Sof(C9B)=Sof(H9B)=Sof(C10B)=0.5*(1-FVAR(2))
 Sof(O1A)=Sof(O3A)=Sof(O2A)=Sof(O4A)=Sof(N10A)=Sof(N12A)=Sof(N9A)=Sof(N3A)=
 Sof(N11A)=Sof(N6A)=Sof(N4A)=Sof(N5A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=
 Sof(C20A)=Sof(C15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C2A)=Sof(H2A)=
 Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(C6A)=Sof(C7A)=Sof(H7A)=
 Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C12A)=Sof(H12A)=
 Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=0.5*FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C18A(H18A), C19A(H19A), C16A(H16A), C17A(H17A), C13B(H13B), C2A(H2A),
 C2B(H2B), C3A(H3A), C3B(H3B), C12B(H12B), C4A(H4A), C20B(H20B), C19B(H19B),
 C18B(H18B), C17B(H17B), C4B(H4B), C7A(H7A), C8A(H8A), C9A(H9A), C10A(H10A),
 C14B(H14B), C12A(H12A), C13A(H13A), C14A(H14A), C6B(H6B), C7B(H7B), C8B(H8B),
 C9B(H9B)
6.b Fitted hexagon refined as free rotating group:
 C18A(C19A,C20A,C15A,C16A,C17A), C20B(C19B,C18B,C17B,C16B,C15B), C5A(C6A,C7A,
 C8A,C9A,C10A), C5B(C6B,C7B,C8B,C9B,C10B)
;
_shelx_res_checksum              39116
_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
;