Reversible guest-induced gate-opening with multiplex spin crossover responses in two-dimensional Hofmann Clathrates
Turo-Cortés, Rubén; Bartual-Murgui, Carlos; Castells-Gil, Javier; Muñoz, Carmen; Martí-Gastaldo, Carlos; Real Cabezos, José Antonio A; Chemical Science  (2020) –; doi:10.1039/D0SC04246C

data_1559162
_publ_section_title
;
 Reversible guest-induced gate-opening with multiplex spin crossover
 responses in two-dimensional Hofmann Clathrates
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC04246C
_journal_year                    2020
_chemical_formula_moiety         'C12 H10 Fe N10 Pt, C0.8 O0.4'
_chemical_formula_sum            'C12.8 H10 Fe N10 O0.4 Pt'
_chemical_formula_weight         561.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-09-17 deposited with the CCDC.	2020-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.922(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9798(16)
_cell_length_b                   7.3662(6)
_cell_length_c                   16.181(2)
_cell_measurement_reflns_used    1612
_cell_measurement_temperature    260.00(10)
_cell_measurement_theta_max      28.6130
_cell_measurement_theta_min      3.9470
_cell_volume                     1784.5(3)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      260.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.852
_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    -93.00 -64.00   1.00    5.00    --  -17.88-178.00 150.00   29
  2  \w     57.00  95.00   1.00    5.00    --   18.67-173.00-120.00   38
  3  \w     29.00  74.00   1.00    5.00    --   18.67   0.00 -60.00   45
  4  \w     11.00  85.00   1.00    5.00    --   18.67  57.00  60.00   74
  5  \w    -52.00  12.00   1.00    5.00    --   18.67   0.00 -60.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0117514000
_diffrn_orient_matrix_UB_12      0.0827287000
_diffrn_orient_matrix_UB_13      0.0191867000
_diffrn_orient_matrix_UB_21      0.0161214000
_diffrn_orient_matrix_UB_22      -0.0342897000
_diffrn_orient_matrix_UB_23      0.0386858000
_diffrn_orient_matrix_UB_31      0.0429663000
_diffrn_orient_matrix_UB_32      0.0353734000
_diffrn_orient_matrix_UB_33      -0.0077037000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4353
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.087
_diffrn_reflns_theta_min         3.647
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.664
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48136
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         7.095
_refine_diff_density_min         -3.452
_refine_diff_density_rms         0.392
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2191
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1006P)^2^+63.5736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.1870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1902
_reflns_number_total             2191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04246c2.cif
_cod_data_source_block           rt457_fenh2pymptetoh_260ka_2
_cod_original_formula_sum        'C12.80 H10 Fe N10 O0.40 Pt'
_cod_database_code               1559162
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.356
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H,H) groups
2. Restrained distances
 N8-H8A
 0.9 with sigma of 0.0001
 N8-H8B
 0.9 with sigma of 0.0001
 N3-H3B
 0.9 with sigma of 0.0001
 H3A-N3
 0.9 with sigma of 0.0001
 H8A-H8B
 1.5 with sigma of 0.0001
 H8B-O1_$1
 2.2 with sigma of 0.0001
 H3A-H3B
 1.5 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(N2) = Uanis(C4) =
Uanis(N3)
Uanis(N6) = Uanis(C10) = Uanis(N7) = Uanis(C9) = Uanis(C8) = Uanis(C7) =
Uanis(N8)
4. Others
 Fixed Sof: H8B(0.5) O1(0.2) C11(0.4)
5.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C1(H1), C3(H3), C7(H7), C4(H4), C10(H10)
;
_shelx_res_checksum              30658
_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 1.710
_oxdiff_exptl_absorpt_empirical_full_min 0.583