#------------------------------------------------------------------------------
#$Date: 2020-09-23 04:13:24 +0300 (Wed, 23 Sep 2020) $
#$Revision: 256637 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/91/1559153.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_1559153
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         'C12 H9 Fe N10 Pd, H3 O'
_chemical_formula_sum            'C12 H12 Fe N10 O Pd'
_chemical_formula_weight         474.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 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                 131.372(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.092(3)
_cell_length_b                   7.0553(10)
_cell_length_c                   14.535(2)
_cell_measurement_reflns_used    3191
_cell_measurement_temperature    120.02
_cell_measurement_theta_max      29.08
_cell_measurement_theta_min      2.57
_cell_volume                     1623.2(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9420
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.259
_diffrn_reflns_theta_min         2.574
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.027
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1101 before and 0.0706 after correction. The Ratio of minimum to maximum transmission is 0.6968. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.606
_refine_diff_density_min         -2.305
_refine_diff_density_rms         0.275
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2266
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0176P)²+78.1367P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1699
_reflns_number_total             2266
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc04246c2.cif
_cod_data_source_block           rt235_fe5apympd_120k_0m
_cod_original_cell_volume        1623.1(4)
_cod_database_code               1559153
_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   0.905
_shelx_estimated_absorpt_t_min   0.687
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
 At 1.5 times of:
  All N(H,H) groups
2. Restrained distances
 H8A-N8
 0.9 with sigma of 0.0001
 O1-H1B
 0.9 with sigma of 0.0001
 H1A-O1
 0.9 with sigma of 0.0001
 N8-H8B
 0.9 with sigma of 0.0001
 H3A-N3
 0.9 with sigma of 0.0001
 N3-H3B
 0.9 with sigma of 0.0001
 H1A-H1B
 1.45 with sigma of 0.0001
 N2_$3-H1B
 2 with sigma of 0.0001
 H8A-H8B
 1.5 with sigma of 0.0001
 H3A-H3B
 1.5 with sigma of 0.0001
 N7_$1-H3B_$2
 2.2 with sigma of 0.0001
3. Others
 Fixed Sof: H3B(0.5) O1(0.5) H1B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C9(H9), C10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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 0.48360(5) 0.500000 0.73519(7) 0.0178(2) Uani 1 2 d S T P . .
Fe1 Fe 0.500000 0.000000 0.500000 0.0160(4) Uani 1 4 d S T P . .
Fe2 Fe 0.500000 1.000000 1.000000 0.0151(4) Uani 1 4 d S T P . .
N1 N 0.3739(6) 0.000000 0.3762(8) 0.0229(19) Uani 1 2 d S T P . .
N2 N 0.24513(19) 0.000000 0.3392(2) 0.053(4) Uani 1 2 d S T P . .
N3 N 0.19562(11) 0.000000 0.0507(2) 0.045(3) Uani 1 2 d DS T P . .
H3A H 0.13882(10) 0.000000 -0.0067(3) 0.067 Uiso 1 2 d DS U P . .
H3B H 0.21985(10) 0.0572(8) 0.02530(18) 0.067 Uiso 0.5 1 d D U P . .
N4 N 0.4975(4) 0.1934(9) 0.5927(5) 0.0173(12) Uani 1 1 d . . . . .
N5 N 0.4813(4) 0.8065(8) 0.8899(5) 0.0190(12) Uani 1 1 d . . . . .
N6 N 0.3766(6) 1.000000 0.9167(9) 0.025(2) Uani 1 2 d S T P . .
N7 N 0.27357(16) 1.000000 0.9400(2) 0.039(3) Uani 1 2 d S T P . .
N8 N 0.16790(9) 1.000000 0.61972(14) 0.058(4) Uani 1 2 d DS T P . .
H8A H 0.11408(10) 1.000000 0.5881(2) 0.087 Uiso 1 2 d DS U P . .
H8B H 0.17192(12) 1.000000 0.56181(17) 0.087 Uiso 1 2 d DS U P . .
C1 C 0.3295(8) 0.000000 0.2565(11) 0.027(2) Uani 1 2 d S T P . .
H1 H 0.358312 0.000000 0.226788 0.033 Uiso 1 2 calc R U P . .
C2 C 0.2393(7) 0.000000 0.1708(11) 0.026(2) Uani 1 2 d S T P . .
C3 C 0.1991(8) 0.000000 0.2173(12) 0.033(3) Uani 1 2 d S T P . .
C4 C 0.3294(8) 0.000000 0.4118(12) 0.036(3) Uani 1 2 d S T P . .
H4 H 0.360891 0.000000 0.497665 0.043 Uiso 1 2 calc R U P . .
C5 C 0.4928(4) 0.3021(10) 0.6465(6) 0.0146(13) Uani 1 1 d . . . . .
C6 C 0.4789(4) 0.6977(10) 0.8294(6) 0.0166(13) Uani 1 1 d . . . . .
C7 C 0.3161(8) 1.000000 0.7982(11) 0.032(3) Uani 1 2 d S T P . .
H7 H 0.330141 1.000000 0.748089 0.038 Uiso 1 2 calc R U P . .
C8 C 0.2296(7) 1.000000 0.7414(11) 0.029(2) Uani 1 2 d S T P . .
C9 C 0.2132(8) 1.000000 0.8209(11) 0.032(3) Uani 1 2 d S T P . .
H9 H 0.156189 1.000000 0.786638 0.038 Uiso 1 2 calc R U P . .
C10 C 0.3542(8) 1.000000 0.9850(12) 0.031(3) Uani 1 2 d S T P . .
H10 H 0.398517 1.000000 1.071628 0.038 Uiso 1 2 calc R U P . .
O1 O 0.2677(2) 0.3646(6) 0.49390(19) 0.072(5) Uiso 0.5 1 d D . P A -1
H1A H 0.2283(2) 0.2742(5) 0.4645(4) 0.087 Uiso 1 1 d D U . . .
H1B H 0.28739(17) 0.3969(6) 0.56875(17) 0.087 Uiso 0.5 1 d D U P . .
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'
O O 0.0106 0.0060 '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
C5 Pd1 C5 88.9(4) 6_565 . ?
C5 Pd1 C6 177.9(3) 6_565 6_565 ?
C5 Pd1 C6 91.4(3) . 6_565 ?
C5 Pd1 C6 91.4(3) 6_565 . ?
C5 Pd1 C6 177.9(3) . . ?
C6 Pd1 C6 88.3(4) 6_565 . ?
N1 Fe1 N1 180.0 5_656 . ?
N4 Fe1 N1 89.7(3) 5_656 5_656 ?
N4 Fe1 N1 89.7(3) 2_656 5_656 ?
N4 Fe1 N1 90.3(3) 2_656 . ?
N4 Fe1 N1 90.3(3) 5_656 . ?
N4 Fe1 N1 90.3(3) . 5_656 ?
N4 Fe1 N1 90.3(3) 6 5_656 ?
N4 Fe1 N1 89.7(3) 6 . ?
N4 Fe1 N1 89.7(3) . . ?
N4 Fe1 N4 90.8(3) . 2_656 ?
N4 Fe1 N4 89.2(3) . 6 ?
N4 Fe1 N4 89.2(3) 5_656 2_656 ?
N4 Fe1 N4 90.8(3) 5_656 6 ?
N4 Fe1 N4 180.0 . 5_656 ?
N4 Fe1 N4 180.0 6 2_656 ?
N5 Fe2 N5 89.7(3) 5_677 2_657 ?
N5 Fe2 N5 90.3(4) 5_677 6_575 ?
N5 Fe2 N5 180.0 6_575 2_657 ?
N5 Fe2 N5 180.0 5_677 . ?
N5 Fe2 N5 89.7(3) 6_575 . ?
N5 Fe2 N5 90.3(4) 2_657 . ?
N5 Fe2 N6 88.5(3) 6_575 5_677 ?
N5 Fe2 N6 88.5(3) 2_657 . ?
N5 Fe2 N6 91.5(3) 2_657 5_677 ?
N5 Fe2 N6 91.5(3) 5_677 5_677 ?
N5 Fe2 N6 91.5(3) . . ?
N5 Fe2 N6 91.5(3) 6_575 . ?
N5 Fe2 N6 88.5(3) 5_677 . ?
N5 Fe2 N6 88.5(3) . 5_677 ?
N6 Fe2 N6 180.0 . 5_677 ?
C1 N1 Fe1 123.3(8) . . ?
C1 N1 C4 116.1(10) . . ?
C4 N1 Fe1 120.6(8) . . ?
C4 N2 C3 117.6(8) . . ?
H3A N3 H3B 112.89(2) . . ?
H3A N3 H3B 112.88(2) . 6 ?
H3B N3 H3B 53.3(8) . 6 ?
C2 N3 H3A 124.0(5) . . ?
C2 N3 H3B 116.7(5) . . ?
C2 N3 H3B 116.7(5) . 6 ?
C5 N4 Fe1 176.4(5) . . ?
C6 N5 Fe2 172.3(6) . . ?
C7 N6 Fe2 122.8(9) . . ?
C7 N6 C10 117.4(11) . . ?
C10 N6 Fe2 119.8(8) . . ?
C9 N7 C10 116.8(8) . . ?
H8A N8 H8B 112.89(2) . . ?
C8 N8 H8A 118.2(5) . . ?
C8 N8 H8B 128.9(5) . . ?
N1 C1 H1 119.2 . . ?
N1 C1 C2 121.6(10) . . ?
C2 C1 H1 119.2 . . ?
N3 C2 C1 120.8(9) . . ?
N3 C2 C3 121.5(10) . . ?
C3 C2 C1 117.7(11) . . ?
N2 C3 C2 120.0(11) . . ?
N1 C4 N2 126.9(11) . . ?
N1 C4 H4 116.5 . . ?
N2 C4 H4 116.5 . . ?
N4 C5 Pd1 177.5(6) . . ?
N5 C6 Pd1 175.5(7) . . ?
N6 C7 H7 119.1 . . ?
N6 C7 C8 121.8(12) . . ?
C8 C7 H7 119.1 . . ?
N8 C8 C7 121.5(10) . . ?
N8 C8 C9 122.3(10) . . ?
C9 C8 C7 116.2(11) . . ?
N7 C9 C8 122.3(11) . . ?
N7 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
N6 C10 N7 125.4(11) . . ?
N6 C10 H10 117.3 . . ?
N7 C10 H10 117.3 . . ?
H1A O1 H1B 107.328(18) . . ?
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 C5 1.994(6) 6_565 ?
Pd1 C5 1.994(6) . ?
Pd1 C6 2.003(7) 6_565 ?
Pd1 C6 2.003(7) . ?
Fe1 N1 1.996(9) . ?
Fe1 N1 1.996(9) 5_656 ?
Fe1 N4 1.943(6) 5_656 ?
Fe1 N4 1.943(6) . ?
Fe1 N4 1.943(6) 2_656 ?
Fe1 N4 1.943(6) 6 ?
Fe2 N5 1.935(6) . ?
Fe2 N5 1.935(6) 2_657 ?
Fe2 N5 1.935(6) 5_677 ?
Fe2 N5 1.935(6) 6_575 ?
Fe2 N6 2.019(10) . ?
Fe2 N6 2.019(10) 5_677 ?
N1 C1 1.324(14) . ?
N1 C4 1.339(14) . ?
N2 C3 1.345(13) . ?
N2 C4 1.339(12) . ?
N3 H3A 0.90000(18) . ?
N3 H3B 0.89999(13) 6 ?
N3 H3B 0.90000(13) . ?
N3 C2 1.331(12) . ?
N4 C5 1.146(8) . ?
N5 C6 1.143(9) . ?
N6 C7 1.300(15) . ?
N6 C10 1.351(14) . ?
N7 C9 1.306(12) . ?
N7 C10 1.361(12) . ?
N8 H8A 0.90000(19) . ?
N8 H8B 0.90000(16) . ?
N8 C8 1.334(13) . ?
C1 H1 0.9500 . ?
C1 C2 1.427(16) . ?
C2 C3 1.390(17) . ?
C4 H4 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.422(17) . ?
C8 C9 1.408(17) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
O1 H1A 0.90000(15) . ?
O1 H1B 0.90000(17) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N1 C1 C2 180.000(2) . . . . ?
Fe1 N1 C4 N2 180.000(2) . . . . ?
Fe2 N6 C7 C8 180.000(6) . . . . ?
Fe2 N6 C10 N7 180.000(4) . . . . ?
N1 C1 C2 N3 180.000(3) . . . . ?
N1 C1 C2 C3 0.000(3) . . . . ?
N3 C2 C3 N2 180.000(1) . . . . ?
N6 C7 C8 N8 180.000(7) . . . . ?
N6 C7 C8 C9 0.000(9) . . . . ?
N8 C8 C9 N7 180.000(5) . . . . ?
C1 N1 C4 N2 0.000(2) . . . . ?
C1 C2 C3 N2 0.000(2) . . . . ?
C3 N2 C4 N1 0.000(4) . . . . ?
C4 N1 C1 C2 0.000(3) . . . . ?
C4 N2 C3 C2 0.000(2) . . . . ?
C7 N6 C10 N7 0.000(9) . . . . ?
C7 C8 C9 N7 0.000(7) . . . . ?
C9 N7 C10 N6 0.000(6) . . . . ?
C10 N6 C7 C8 0.000(9) . . . . ?
C10 N7 C9 C8 0.000(8) . . . . ?
