#------------------------------------------------------------------------------
#$Date: 2020-09-23 04:13:24 +0300 (Wed, 23 Sep 2020) $
#$Revision: 256637 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/91/1559150.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1559150
loop_
_publ_author_name
'Turo-Cortés, Rubén'
'Bartual-Murgui, Carlos'
'Castells-Gil, Javier'
'Muñoz, Carmen'
'Martí-Gastaldo, Carlos'
'Real Cabezos, José Antonio A'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -59.00  43.00   1.00   15.00    --  -15.20  19.00 -30.00  102
  2  ω    -43.00 -18.00   1.00   15.00    --  -15.20  77.00 150.00   25
  3  ω      9.00  51.00   1.00   15.00    --  -15.20  77.00 150.00   42
  4  ω    -85.00  15.00   1.00   15.00    --  -15.20 -77.00  30.00  100
  5  ω    -12.00  22.00   1.00   15.00    --  -15.20 -99.00 -90.00   34
  6  ω     -4.00  31.00   1.00   15.00    --   15.98  57.00 -60.00   35
  7  ω     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       'ω 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/[σ²(Fo²)+(0.0403P)²+73.0831P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.54979(9) 1.250000 0.22945(9) 0.0215(4) Uani 1 2 d S T P . .
Fe1 Fe 0.79573(17) 0.750000 0.30759(18) 0.0221(6) Uani 1 2 d S T P . .
N1 N 0.7670(13) 0.750000 0.4417(11) 0.0423(19) Uani 1 2 d S T P . .
N2 N 0.8056(16) 0.750000 0.1679(14) 0.057(2) Uani 1 2 d S T P . .
N3 N 0.6907(8) 0.9552(15) 0.2925(7) 0.028(2) Uani 1 1 d . . . . .
N4 N 0.4019(8) 1.5481(16) 0.1855(8) 0.035(3) Uani 1 1 d . . . . .
N5 N 0.8157(13) 0.750000 0.5839(11) 0.0423(19) Uani 1 2 d S T P . .
N6 N 0.5602(12) 0.750000 0.5769(11) 0.0423(19) Uani 1 2 d S T P . .
H6A H 0.540438 0.640090 0.581032 0.051 Uiso 0.5 1 d GR . . . .
H6B H 0.553466 0.803750 0.624594 0.051 Uiso 0.5 1 d GR . . . .
N7 N 0.9021(16) 0.750000 0.0447(14) 0.057(2) Uani 1 2 d S T P . .
N8 N 0.6532(16) 0.750000 -0.0160(15) 0.057(2) Uani 1 2 d S T P . .
H8A H 0.662646 0.683376 -0.060522 0.068 Uiso 0.5 1 d GR . . . .
H8B H 0.604936 0.706605 0.010918 0.068 Uiso 0.5 1 d GR . . . .
C1 C 0.6808(16) 0.750000 0.4686(13) 0.0423(19) Uani 1 2 d S T P . .
H1 H 0.632909 0.750000 0.429020 0.051 Uiso 1 2 calc RS T P . .
C2 C 0.6560(16) 0.750000 0.5538(13) 0.0423(19) Uani 1 2 d S T P . .
C3 C 0.7299(15) 0.750000 0.6070(14) 0.0423(19) Uani 1 2 d S T P . .
H3 H 0.717489 0.750000 0.664335 0.051 Uiso 1 2 calc RS T P . .
C4 C 0.8322(16) 0.750000 0.5045(13) 0.0423(19) Uani 1 2 d S T P . .
H4 H 0.894792 0.750000 0.488254 0.051 Uiso 1 2 calc RS T P . .
C5 C 0.732(2) 0.750000 0.1137(18) 0.057(2) Uani 1 2 d S T P . .
H5 H 0.672696 0.750000 0.138214 0.068 Uiso 1 2 calc RS T P . .
C6 C 0.734(2) 0.750000 0.0366(18) 0.057(2) Uani 1 2 d S T P . .
C7 C 0.8228(19) 0.750000 -0.0028(18) 0.057(2) Uani 1 2 d S T P . .
H7 H 0.827085 0.750000 -0.061047 0.068 Uiso 1 2 calc RS T P . .
C8 C 0.888(2) 0.750000 0.1262(17) 0.057(2) Uani 1 2 d S T P . .
H8 H 0.941552 0.750000 0.159434 0.068 Uiso 1 2 calc RS T P . .
C9 C 0.6383(8) 1.0610(16) 0.2704(8) 0.023(2) Uani 1 1 d . . . . .
C10 C 0.4577(9) 1.4410(17) 0.1976(8) 0.025(3) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 Pd1 C9 88.9(7) . 7_585 ?
C9 Pd1 C10 175.5(5) 7_585 7_585 ?
C9 Pd1 C10 175.5(5) . . ?
C9 Pd1 C10 90.3(5) . 7_585 ?
C9 Pd1 C10 90.3(5) 7_585 . ?
C10 Pd1 C10 90.1(7) . 7_585 ?
N1 Fe1 N2 172.8(8) . . ?
N3 Fe1 N1 88.7(5) . . ?
N3 Fe1 N1 88.7(5) 7_575 . ?
N3 Fe1 N2 86.1(5) . . ?
N3 Fe1 N2 86.1(5) 7_575 . ?
N3 Fe1 N3 89.9(6) 7_575 . ?
N4 Fe1 N1 94.8(5) 6_646 . ?
N4 Fe1 N1 94.8(5) 4_575 . ?
N4 Fe1 N2 90.4(5) 6_646 . ?
N4 Fe1 N2 90.4(5) 4_575 . ?
N4 Fe1 N3 90.5(4) 6_646 7_575 ?
N4 Fe1 N3 176.5(5) 6_646 . ?
N4 Fe1 N3 176.5(5) 4_575 7_575 ?
N4 Fe1 N3 90.5(4) 4_575 . ?
N4 Fe1 N4 88.9(6) 4_575 6_646 ?
C1 N1 Fe1 120.1(15) . . ?
C1 N1 C4 113.7(19) . . ?
C4 N1 Fe1 126.2(15) . . ?
C5 N2 Fe1 125.7(19) . . ?
C8 N2 Fe1 123.1(18) . . ?
C8 N2 C5 111(2) . . ?
C9 N3 Fe1 168.4(11) . . ?
C10 N4 Fe1 167.2(12) . 6_566 ?
C3 N5 C4 117(2) . . ?
C8 N7 C7 115(2) . . ?
N1 C1 C2 124(2) . . ?
C1 C2 N6 120(2) . . ?
C3 C2 N6 126(2) . . ?
C3 C2 C1 114(2) . . ?
N5 C3 C2 125(2) . . ?
N5 C4 N1 126(2) . . ?
C6 C5 N2 128(3) . . ?
C5 C6 N8 125(3) . . ?
C5 C6 C7 117(3) . . ?
C7 C6 N8 118(2) . . ?
N7 C7 C6 120(3) . . ?
N7 C8 N2 128(3) . . ?
N3 C9 Pd1 178.2(12) . . ?
N4 C10 Pd1 174.6(12) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C9 1.993(12) . ?
Pd1 C9 1.993(12) 7_585 ?
Pd1 C10 1.993(13) 7_585 ?
Pd1 C10 1.993(13) . ?
Fe1 N1 2.174(18) . ?
Fe1 N2 2.23(2) . ?
Fe1 N3 2.145(11) . ?
Fe1 N3 2.145(11) 7_575 ?
Fe1 N4 2.129(11) 4_575 ?
Fe1 N4 2.129(11) 6_646 ?
N1 C1 1.30(3) . ?
N1 C4 1.37(3) . ?
N2 C5 1.36(3) . ?
N2 C8 1.35(3) . ?
N3 C9 1.136(15) . ?
N4 C10 1.139(16) . ?
N5 C3 1.28(3) . ?
N5 C4 1.29(3) . ?
N6 C2 1.42(3) . ?
N7 C7 1.36(3) . ?
N7 C8 1.31(3) . ?
N8 C6 1.42(3) . ?
C1 C2 1.40(3) . ?
C2 C3 1.35(3) . ?
C5 C6 1.23(4) . ?
C6 C7 1.42(4) . ?
