#------------------------------------------------------------------------------
#$Date: 2020-09-23 04:13:24 +0300 (Wed, 23 Sep 2020) $
#$Revision: 256637 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/91/1559158.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_1559158
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 H10 Fe N10 Pd, H2 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                 131.494(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.454(3)
_cell_length_b                   7.1986(8)
_cell_length_c                   14.7221(16)
_cell_measurement_reflns_used    3862
_cell_measurement_temperature    180.01
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      2.53
_cell_volume                     1703.0(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      180.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.937
_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  0.0617
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10741
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.971
_diffrn_reflns_theta_min         2.535
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.932
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1086 before and 0.0724 after correction.
The Ratio of minimum to maximum transmission is 0.6865.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.851
_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         2.003
_refine_diff_density_min         -1.608
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2496
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0445P)²+42.1677P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1942
_reflns_number_total             2496
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc04246c2.cif
_cod_data_source_block           rt235_fe5apympd_180k_0m
_cod_original_cell_volume        1703.0(3)
_cod_database_code               1559158
_shelx_shelxl_version_number     2018/3
_publcif_funding_html
;
;
_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   0.910
_shelx_estimated_absorpt_t_min   0.699
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1-H1b
 0.9 with sigma of 0.0001
 H8b_$1-N8
 0.9 with sigma of 0.0001
 N8-H8a
 0.9 with sigma of 0.0001
 O1-H1a
 0.9 with sigma of 0.0001
 H3b-N3
 0.9 with sigma of 0.0001
 N3-H3a
 0.9 with sigma of 0.0001
 H8a-H8b_$1
 1.5 with sigma of 0.0001
 H8a-O1_$2
 2.1 with sigma of 0.0001
 H1b-H1a
 1.45 with sigma of 0.0001
 H1b-N2
 2 with sigma of 0.0001
 H3b-H3a
 1.5 with sigma of 0.0001
3. Others
 Fixed Sof: O1(0.5) H1a(0.5) H1b(0.5) H3a(0.5) H3b(0.5) H8b(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), 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 0.51479(4) 0.500000 0.77095(6) 0.02099(19) Uani 1 2 d S T P . .
Fe1 Fe 0.500000 1.000000 1.000000 0.0193(3) Uani 1 4 d S T P . .
Fe2 Fe 0.500000 0.000000 0.500000 0.0196(3) Uani 1 4 d S T P . .
O1 O 0.22793(13) 1.1108(4) 1.01296(15) 0.079(4) Uiso 0.5 1 d D . P A -1
H1A H 0.2624(3) 1.2093(4) 1.0449(3) 0.119 Uiso 0.5 1 d D U P B -1
H1B H 0.21867(15) 1.0765(6) 0.94610(15) 0.119 Uiso 0.5 1 d D U P C -1
N1 N 0.3742(5) 1.000000 0.8817(7) 0.0268(15) Uani 1 2 d S T P . .
N2 N 0.25173(17) 1.000000 0.8525(2) 0.044(2) Uani 1 2 d DS T P . .
N3 N 0.19546(13) 1.000000 0.5612(2) 0.050(3) Uani 1 2 d DS T P . .
H3A H 0.22641(11) 0.981(2) 0.5410(2) 0.060 Uiso 0.5 1 d D U P . .
H3B H 0.14316(13) 0.9568(9) 0.5051(4) 0.060 Uiso 0.5 1 d D U P . .
N4 N 0.4999(3) 0.8076(7) 0.9067(4) 0.0238(10) Uani 1 1 d . . . . .
N5 N 0.5242(4) 0.2062(7) 0.6239(5) 0.0288(11) Uani 1 1 d . . . . .
N6 N 0.3696(5) 0.000000 0.4201(7) 0.0284(16) Uani 1 2 d S T P . .
N7 N 0.2710(6) 0.000000 0.4475(8) 0.045(2) Uani 1 2 d S T P . .
N8 N 0.16163(12) 0.000000 0.1272(2) 0.059(3) Uani 1 2 d DS T P . .
H8A H 0.18913(10) 0.000000 0.10048(15) 0.071 Uiso 1 2 d DS U P . .
H8B H 0.12546(14) -0.0949(3) 0.0973(3) 0.071 Uiso 0.5 1 d . U P . .
C1 C 0.3296(6) 1.000000 0.7633(8) 0.0285(18) Uani 1 2 d S T P . .
H1 H 0.356889 1.000000 0.732386 0.034 Uiso 1 2 calc R U P . .
C2 C 0.2415(7) 1.000000 0.6817(9) 0.036(2) Uani 1 2 d S T P . .
C3 C 0.2045(7) 1.000000 0.7332(10) 0.038(2) Uani 1 2 d S T P . .
H3 H 0.145606 1.000000 0.682033 0.046 Uiso 1 2 calc R U P . .
C4 C 0.3343(7) 1.000000 0.9227(10) 0.037(2) Uani 1 2 d S T P . .
H4 H 0.367113 1.000000 1.008049 0.044 Uiso 1 2 calc R U P . .
C5 C 0.5044(4) 0.6969(7) 0.8557(5) 0.0205(11) Uani 1 1 d . . . . .
C6 C 0.5224(4) 0.3088(8) 0.6813(5) 0.0222(11) Uani 1 1 d . . . . .
C7 C 0.3086(7) 0.000000 0.3025(9) 0.034(2) Uani 1 2 d S T P . .
H7 H 0.321339 0.000000 0.251853 0.041 Uiso 1 2 calc R U P . .
C8 C 0.2242(6) 0.000000 0.2483(9) 0.034(2) Uani 1 2 d S T P . .
C9 C 0.2099(7) 0.000000 0.3279(10) 0.040(2) Uani 1 2 d S T P . .
H9 H 0.154054 0.000000 0.295068 0.048 Uiso 1 2 calc R U P . .
C10 C 0.3491(7) 0.000000 0.4895(10) 0.041(2) Uani 1 2 d S T P . .
H10 H 0.393544 0.000000 0.574957 0.049 Uiso 1 2 calc R 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 90.4(3) 6_565 . ?
C6 Pd1 C5 178.0(2) . . ?
C6 Pd1 C5 178.0(2) 6_565 6_565 ?
C6 Pd1 C5 90.9(2) 6_565 . ?
C6 Pd1 C5 90.9(2) . 6_565 ?
C6 Pd1 C6 87.6(3) 6_565 . ?
N1 Fe1 N1 180.0(4) 5_677 . ?
N4 Fe1 N1 89.1(2) 6_575 5_677 ?
N4 Fe1 N1 90.9(2) 5_677 5_677 ?
N4 Fe1 N1 90.9(2) . . ?
N4 Fe1 N1 89.1(2) 2_657 . ?
N4 Fe1 N1 90.9(2) 2_657 5_677 ?
N4 Fe1 N1 89.1(2) . 5_677 ?
N4 Fe1 N1 90.9(2) 6_575 . ?
N4 Fe1 N1 89.1(2) 5_677 . ?
N4 Fe1 N4 89.5(3) 5_677 6_575 ?
N4 Fe1 N4 180.0 6_575 2_657 ?
N4 Fe1 N4 90.5(3) . 6_575 ?
N4 Fe1 N4 90.5(3) 5_677 2_657 ?
N4 Fe1 N4 89.5(3) . 2_657 ?
N4 Fe1 N4 180.0(3) . 5_677 ?
N5 Fe2 N5 180.0 6 2_656 ?
N5 Fe2 N5 91.7(3) 5_656 6 ?
N5 Fe2 N5 88.3(3) 5_656 2_656 ?
N5 Fe2 N5 180.0 5_656 . ?
N5 Fe2 N5 88.3(3) 6 . ?
N5 Fe2 N5 91.7(3) 2_656 . ?
N5 Fe2 N6 87.7(2) 5_656 5_656 ?
N5 Fe2 N6 87.7(2) 2_656 5_656 ?
N5 Fe2 N6 87.7(2) 6 . ?
N5 Fe2 N6 92.3(2) 2_656 . ?
N5 Fe2 N6 87.7(2) . . ?
N5 Fe2 N6 92.3(2) . 5_656 ?
N5 Fe2 N6 92.3(2) 6 5_656 ?
N5 Fe2 N6 92.3(2) 5_656 . ?
N6 Fe2 N6 180.0 5_656 . ?
H1A O1 H1B 107.328(18) . . ?
C1 N1 Fe1 121.6(6) . . ?
C1 N1 C4 118.4(9) . . ?
C4 N1 Fe1 120.0(7) . . ?
C3 N2 C4 118.9(7) . . ?
H3A N3 H3A 17(2) . 6_575 ?
H3A N3 H3B 112.89(2) . . ?
H3A N3 H3B 119.6(8) . 6_575 ?
H3A N3 H3B 112.89(2) 6_575 6_575 ?
H3B N3 H3A 119.6(8) . 6_575 ?
H3B N3 H3B 40.5(9) . 6_575 ?
C2 N3 H3A 112.3(5) . . ?
C2 N3 H3A 112.3(5) . 6_575 ?
C2 N3 H3B 126.2(6) . 6_575 ?
C2 N3 H3B 126.2(6) . . ?
C5 N4 Fe1 176.2(5) . . ?
C6 N5 Fe2 167.1(5) . . ?
C7 N6 Fe2 120.7(7) . . ?
C7 N6 C10 117.3(9) . . ?
C10 N6 Fe2 122.0(7) . . ?
C9 N7 C10 116.3(9) . . ?
H8A N8 H8B 112.89(2) . 6 ?
H8A N8 H8B 112.89(2) . . ?
H8B N8 H8B 98.8(5) . 6 ?
C8 N8 H8A 102.2(5) . . ?
C8 N8 H8B 115.4(3) . 6 ?
C8 N8 H8B 115.4(3) . . ?
N1 C1 H1 119.6 . . ?
N1 C1 C2 120.8(9) . . ?
C2 C1 H1 119.6 . . ?
N3 C2 C1 121.3(9) . . ?
N3 C2 C3 121.7(9) . . ?
C3 C2 C1 116.9(9) . . ?
N2 C3 C2 120.2(9) . . ?
N2 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
N1 C4 N2 124.8(9) . . ?
N1 C4 H4 117.6 . . ?
N2 C4 H4 117.6 . . ?
N4 C5 Pd1 178.4(6) . . ?
N5 C6 Pd1 175.8(5) . . ?
N6 C7 H7 118.9 . . ?
N6 C7 C8 122.2(9) . . ?
C8 C7 H7 118.9 . . ?
N8 C8 C7 122.0(8) . . ?
N8 C8 C9 122.1(9) . . ?
C9 C8 C7 115.9(9) . . ?
N7 C9 C8 122.8(10) . . ?
N7 C9 H9 118.6 . . ?
C8 C9 H9 118.6 . . ?
N6 C10 H10 117.3 . . ?
N7 C10 N6 125.5(10) . . ?
N7 C10 H10 117.3 . . ?
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 1.997(5) 6_565 ?
Pd1 C5 1.997(5) . ?
Pd1 C6 1.987(6) 6_565 ?
Pd1 C6 1.987(6) . ?
Fe1 N1 2.022(8) 5_677 ?
Fe1 N1 2.022(8) . ?
Fe1 N4 1.950(5) 6_575 ?
Fe1 N4 1.950(5) 2_657 ?
Fe1 N4 1.950(5) . ?
Fe1 N4 1.950(5) 5_677 ?
Fe2 N5 2.132(5) 5_656 ?
Fe2 N5 2.132(5) . ?
Fe2 N5 2.132(5) 2_656 ?
Fe2 N5 2.132(5) 6 ?
Fe2 N6 2.203(8) 5_656 ?
Fe2 N6 2.203(8) . ?
O1 H1A 0.90000(15) . ?
O1 H1B 0.90000(14) . ?
N1 C1 1.321(11) . ?
N1 C4 1.335(12) . ?
N2 C3 1.324(11) . ?
N2 C4 1.335(11) . ?
N3 H3A 0.90003(18) 6_575 ?
N3 H3A 0.90000(16) . ?
N3 H3B 0.90000(15) . ?
N3 H3B 0.90003(14) 6_575 ?
N3 C2 1.342(10) . ?
N4 C5 1.141(7) . ?
N5 C6 1.142(8) . ?
N6 C7 1.307(12) . ?
N6 C10 1.352(13) . ?
N7 C9 1.327(14) . ?
N7 C10 1.349(14) . ?
N8 H8A 0.90000(13) . ?
N8 H8B 0.90000(13) 6 ?
N8 H8B 0.90000(13) . ?
N8 C8 1.345(10) . ?
C1 H1 0.9500 . ?
C1 C2 1.417(14) . ?
C2 C3 1.414(15) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.413(15) . ?
C8 C9 1.395(14) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
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(5) . . . . ?
Fe1 N1 C4 N2 180.000(3) . . . . ?
Fe2 N6 C7 C8 180.000(2) . . . . ?
Fe2 N6 C10 N7 180.000(3) . . . . ?
N1 C1 C2 N3 180.000(5) . . . . ?
N1 C1 C2 C3 0.000(7) . . . . ?
N3 C2 C3 N2 180.000(3) . . . . ?
N6 C7 C8 N8 180.000(3) . . . . ?
N6 C7 C8 C9 0.000(3) . . . . ?
N8 C8 C9 N7 180.000(3) . . . . ?
C1 N1 C4 N2 0.000(8) . . . . ?
C1 C2 C3 N2 0.000(5) . . . . ?
C3 N2 C4 N1 0.000(8) . . . . ?
C4 N1 C1 C2 0.000(7) . . . . ?
C4 N2 C3 C2 0.000(6) . . . . ?
C7 N6 C10 N7 0.000(5) . . . . ?
C7 C8 C9 N7 0.000(3) . . . . ?
C9 N7 C10 N6 0.000(5) . . . . ?
C10 N6 C7 C8 0.000(3) . . . . ?
C10 N7 C9 C8 0.000(4) . . . . ?
