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_1559150
_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         '0.5(C24 H20 Fe2 N20 Pd2)'
_chemical_formula_sum            'C12 H10 Fe N10 Pd'
_chemical_formula_weight         456.55
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-22 deposited with the CCDC.	2020-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2723(10)
_cell_length_b                   7.3843(5)
_cell_length_c                   15.9189(12)
_cell_measurement_reflns_used    2332
_cell_measurement_temperature    260.00(10)
_cell_measurement_theta_max      22.6110
_cell_measurement_theta_min      3.8140
_cell_volume                     1677.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.930
_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    -59.00  43.00   1.00   15.00    --  -15.20  19.00 -30.00  102
  2  \w    -43.00 -18.00   1.00   15.00    --  -15.20  77.00 150.00   25
  3  \w      9.00  51.00   1.00   15.00    --  -15.20  77.00 150.00   42
  4  \w    -85.00  15.00   1.00   15.00    --  -15.20 -77.00  30.00  100
  5  \w    -12.00  22.00   1.00   15.00    --  -15.20 -99.00 -90.00   34
  6  \w     -4.00  31.00   1.00   15.00    --   15.98  57.00 -60.00   35
  7  \w     36.00  90.00   1.00   15.00    --   15.98-178.00 -90.00   54
;
_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      -0.0059061000
_diffrn_orient_matrix_UB_12      -0.0284015000
_diffrn_orient_matrix_UB_13      -0.0731922000
_diffrn_orient_matrix_UB_21      -0.0492615000
_diffrn_orient_matrix_UB_22      0.0014312000
_diffrn_orient_matrix_UB_23      0.0121297000
_diffrn_orient_matrix_UB_31      -0.0027943000
_diffrn_orient_matrix_UB_32      0.0343138000
_diffrn_orient_matrix_UB_33      -0.0609954000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11692
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.989
_diffrn_reflns_theta_min         3.360
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.953
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.808
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.004
_refine_diff_density_min         -1.545
_refine_diff_density_rms         0.288
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         2021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0902
_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^)+(0.0403P)^2^+73.0831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2291
_refine_ls_wR_factor_ref         0.2483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1419
_reflns_number_total             2021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04246c2.cif
_cod_data_source_block           rt235_260k_des
_cod_database_code               1559150
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.696
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C6) = Uanis(C5) = Uanis(N2) = Uanis(C8) = Uanis(N7) =
Uanis(N8)
Uanis(N1) = Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(N5) = Uanis(C4) =
Uanis(N6)
3. Others
 Fixed Sof: H6A(0.5) H6B(0.5) H8A(0.5) H8B(0.5)
4.a Rotating group:
 N6(H6A,H6B), N8(H8A,H8B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8)
;
_shelx_res_checksum              12266
_olex2_date_sample_data_collection 2019-04-12
_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 2.113
_oxdiff_exptl_absorpt_empirical_full_min 0.648