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_1559160
_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                 92.699(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8483(15)
_cell_length_b                   7.1717(7)
_cell_length_c                   15.880(3)
_cell_measurement_reflns_used    1016
_cell_measurement_temperature    99.5(7)
_cell_measurement_theta_max      27.1560
_cell_measurement_theta_min      4.0760
_cell_volume                     1689.1(4)
_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      99.5(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.862
_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    -90.00 -38.00   1.00    5.00    --  -18.04 178.00  60.00   52
  2  \w    -40.00  -1.00   1.00    5.00    --  -18.04 -77.00-150.00   39
  3  \w      4.00  32.00   1.00    5.00    --   18.82  77.00 120.00   28
  4  \w    -54.00  52.00   1.00    5.00    --   18.82 -19.00-120.00  106
;
_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      -0.0112584000
_diffrn_orient_matrix_UB_12      0.0862855000
_diffrn_orient_matrix_UB_13      0.0188818000
_diffrn_orient_matrix_UB_21      0.0167813000
_diffrn_orient_matrix_UB_22      -0.0333653000
_diffrn_orient_matrix_UB_23      0.0397051000
_diffrn_orient_matrix_UB_31      0.0433174000
_diffrn_orient_matrix_UB_32      0.0351333000
_diffrn_orient_matrix_UB_33      -0.0081398000
_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  0.0527
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3591
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.938
_diffrn_reflns_theta_min         3.672
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.153
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70140
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.207
_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         14.244
_refine_diff_density_min         -4.872
_refine_diff_density_rms         0.577
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         2079
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.1183
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1097P)^2^+251.2023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2800
_refine_ls_wR_factor_ref         0.2875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1857
_reflns_number_total             2079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04246c2.cif
_cod_data_source_block           rt457_fenh2pymptetoh_100ka_2
_cod_original_cell_volume        1689.2(4)
_cod_original_formula_sum        'C12.80 H10 Fe N10 O0.40 Pt'
_cod_database_code               1559160
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.341
_reflns_odcompleteness_completeness 99.41
_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-H8B
 0.9 with sigma of 0.0001
 N8-H8A
 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
 H8B-O1
 2.2 with sigma of 0.0001
 H8A-H8B
 1.5 with sigma of 0.0001
 H3A-H3B
 1.5 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(N6) = Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(N7) = Uanis(C10) =
Uanis(N8)
Uanis(C4) = Uanis(N1) = Uanis(C2) = Uanis(C3) = Uanis(N2) = Uanis(N3)
4. Others
 Fixed Sof: H8B(0.5) O1(0.2) C11(0.4)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C7(H7), C9(H9), C10(H10)
;
_shelx_res_checksum              90664
_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 1.358
_oxdiff_exptl_absorpt_empirical_full_min 0.763