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_1559165
_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 Pd, 0.5(C H4 O)'
_chemical_formula_sum            'C12.5 H12 Fe N10 O0.5 Pd'
_chemical_formula_weight         472.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0184(12)
_cell_length_b                   32.5156(18)
_cell_length_c                   7.3514(4)
_cell_measurement_reflns_used    911
_cell_measurement_temperature    260.0(2)
_cell_measurement_theta_max      26.7370
_cell_measurement_theta_min      3.9600
_cell_volume                     3589.9(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      260.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.835
_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    -88.00 -62.00   1.00   30.00    --  -14.81-178.00  60.00   26
  2  \w    -57.00  57.00   1.00   30.00    --  -14.81  19.00-180.00  114
;
_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      -0.0162461000
_diffrn_orient_matrix_UB_12      0.0133803000
_diffrn_orient_matrix_UB_13      0.0685554000
_diffrn_orient_matrix_UB_21      -0.0422743000
_diffrn_orient_matrix_UB_22      0.0003913000
_diffrn_orient_matrix_UB_23      -0.0430863000
_diffrn_orient_matrix_UB_31      -0.0135657000
_diffrn_orient_matrix_UB_32      -0.0172113000
_diffrn_orient_matrix_UB_33      0.0523726000
_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  0.0509
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.835
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9664
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.982
_diffrn_reflns_theta_min         3.300
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.830
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93558
_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    1.749
_exptl_crystal_description       plate
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.012
_refine_diff_density_min         -1.507
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3897
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.0816
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+25.2612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2037
_refine_ls_wR_factor_ref         0.2498
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1884
_reflns_number_total             3897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04246c2.cif
_cod_data_source_block           rt312_nh2pympdmeoh_260k
_cod_original_formula_sum        'C12.50 H12 Fe N10 O0.50 Pd'
_cod_database_code               1559165
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.810
_reflns_odcompleteness_completeness 99.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H3A,H3B} of N3
 At 1.5 times of:
  All C(H,H,H) groups, {H11A,H11B} of N11, {H14A,H14B} of N14, {H8A,H8B} of
  N8, All O(H) groups
2. Restrained distances
 O1-C21
 1.4 with sigma of 0.02
 N14-H14A_$1
 0.9 with sigma of 0.0001
 H14B_$1-N14
 0.9 with sigma of 0.0001
 N8-H8B
 0.9 with sigma of 0.0001
 N8-H8A
 0.9 with sigma of 0.0001
 H14B_$1-H14A_$1
 1.5 with sigma of 0.0001
 H14A-O2_$2
 2.2 with sigma of 0.0001
 N11_$1-H11A_$1
 0.9 with sigma of 0.0001
 H11A_$1-H11B_$1
 1.5 with sigma of 0.0001
 N11_$1-H11B_$1
 0.9 with sigma of 0.0001
 H8A-H8B
 1.5 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(N11) = Uanis(C12) = Uanis(C13) = Uanis(N10) = Uanis(C14) = Uanis(N9) =
Uanis(C11)
Uanis(N8) = Uanis(C8) = Uanis(C9) = Uanis(N7) = Uanis(C10) = Uanis(N6) =
Uanis(C7)
Uanis(N14) = Uanis(C16) = Uanis(C15) = Uanis(N12) = Uanis(C18) = Uanis(N13) =
Uanis(C17)
Uanis(N1) = Uanis(C4) = Uanis(N2) = Uanis(C3) = Uanis(C2) = Uanis(C1) =
Uanis(N3)
4. Others
 Fixed Sof: H8B(0.5) H11B(0.5) H14A(0.5) O2(0.25) H2(0.25) C22(0.25)
 H22A(0.25) H22B(0.25) H22C(0.25) O1(0.25) H1A(0.25) C21(0.25) H21A(0.25)
 H21B(0.25) H21C(0.25)
 Fixed X: O2(0.496119) C22(0.484519) O1(1.01363)
 Fixed Y: O2(0.7643) C22(0.762381) O1(0.484839)
 Fixed Z: O2(1.25) C22(1.05867) O1(1.25)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18)
5.b X=CH2 refined with riding coordinates:
 N3(H3A,H3B)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C21(H21A,H21B,H21C)
5.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1A)
;
_shelx_res_checksum              6336
_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 1.212
_oxdiff_exptl_absorpt_empirical_full_min 0.853