#------------------------------------------------------------------------------
#$Date: 2020-09-23 04:13:24 +0300 (Wed, 23 Sep 2020) $
#$Revision: 256637 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/91/1559154.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_1559154
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, 0.5(H4 O2)'
_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                 131.902(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.770(3)
_cell_length_b                   7.3679(8)
_cell_length_c                   14.951(3)
_cell_measurement_reflns_used    4213
_cell_measurement_temperature    260.0
_cell_measurement_theta_max      29.90
_cell_measurement_theta_min      2.51
_cell_volume                     1784.9(5)
_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      260.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.962
_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  0.0555
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11544
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.929
_diffrn_reflns_theta_min         2.514
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.843
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1219 before and 0.0714 after correction.
The Ratio of minimum to maximum transmission is 0.7496.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.766
_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         2.340
_refine_diff_density_min         -1.681
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2671
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0674P)²+24.3621P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2122
_reflns_number_total             2671
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc04246c2.cif
_cod_data_source_block           rt235_fe5apympd_260k_0ma_a
_cod_database_code               1559154
_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   0.913
_shelx_estimated_absorpt_t_min   0.709
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H,H) groups, All O(H,H) groups
2. Restrained distances
 N3-H3A
 0.9 with sigma of 0.0001
 H8A-N8
 0.9 with sigma of 0.0001
 N8-H8B
 0.9 with sigma of 0.0001
 H1B-O1
 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
 O1-H8B
 2.2 with sigma of 0.0001
 H8A-H8B
 1.5 with sigma of 0.0001
 H1B-H1A
 1.45 with sigma of 0.0001
 H3B-H3A
 1.5 with sigma of 0.0001
3. Others
 Fixed Sof: H8A(0.5) H8B(0.5) O1(0.5) H1B(0.5)
 Fixed Uiso: O1(0.08)
4.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1), C9(H9), C7(H7), C4(H4), C3(H3)
;
_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
Pd01 Pd 0.51650(4) 0.500000 0.26458(5) 0.0251(2) Uani 1 2 d S T P . .
Fe2 Fe 0.500000 0.000000 0.000000 0.0247(3) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 1.000000 0.500000 0.0265(3) Uani 1 4 d S T P . .
N4 N 0.5008(3) 0.7955(8) 0.3985(5) 0.0392(12) Uani 1 1 d . . . . .
N5 N 0.5232(3) 0.2044(7) 0.1213(5) 0.0381(11) Uani 1 1 d . . . . .
N6 N 0.3680(5) 0.000000 -0.0862(7) 0.0381(16) Uani 1 2 d S T P . .
C6 C 0.5230(4) 0.3116(8) 0.1775(5) 0.0309(11) Uani 1 1 d . . . . .
N1 N 0.3636(5) 1.000000 0.3652(7) 0.0390(17) Uani 1 2 d S T P . .
C5 C 0.5066(4) 0.6888(8) 0.3484(5) 0.0306(11) Uani 1 1 d . . . . .
N7 N 0.2693(6) 0.000000 -0.0646(10) 0.064(3) Uani 1 2 d S T P . .
N3 N 0.19080(10) 1.000000 0.04633(19) 0.078(4) Uani 1 2 d DS T P . .
H3A H 0.21665(11) 1.000000 0.0182(2) 0.118 Uiso 1 2 d DS U P . .
H3B H 0.13545(9) 1.000000 -0.0126(3) 0.118 Uiso 1 2 d DS U P . .
C2 C 0.2335(6) 1.000000 0.1633(10) 0.046(2) Uani 1 2 d S T P . .
N2 N 0.2384(6) 1.000000 0.3279(10) 0.072(3) Uani 1 2 d S T P . .
C10 C 0.3478(7) 0.000000 -0.0190(10) 0.049(2) Uani 1 2 d S T P . .
H10 H 0.390301 0.000000 0.064167 0.059 Uiso 1 2 calc R U P . .
C1 C 0.3198(6) 1.000000 0.2491(9) 0.042(2) Uani 1 2 d S T P . .
H1 H 0.347797 1.000000 0.221986 0.051 Uiso 1 2 calc R U P . .
C8 C 0.2249(6) 0.000000 -0.2582(10) 0.051(3) Uani 1 2 d S T P . .
C9 C 0.2103(7) 0.000000 -0.1808(11) 0.055(3) Uani 1 2 d S T P . .
H9 H 0.155983 0.000000 -0.213594 0.066 Uiso 1 2 calc R U P . .
C7 C 0.3083(6) 0.000000 -0.2018(9) 0.043(2) Uani 1 2 d S T P . .
H7 H 0.321438 0.000000 -0.249586 0.052 Uiso 1 2 calc R U P . .
C4 C 0.3210(7) 1.000000 0.4016(10) 0.057(3) Uani 1 2 d S T P . .
H4 H 0.351265 1.000000 0.483884 0.068 Uiso 1 2 calc R U P . .
C3 C 0.1952(7) 1.000000 0.2104(11) 0.057(3) Uani 1 2 d S T P . .
H3 H 0.137907 1.000000 0.157752 0.068 Uiso 1 2 calc R U P . .
N8 N 0.16361(12) 0.000000 -0.3776(3) 0.081(4) Uani 1 2 d DS T P . .
H8A H 0.11832(11) 0.0635(5) -0.4062(3) 0.121 Uiso 0.5 1 d D U P . .
H8B H 0.19239(10) 0.0523(8) -0.39412(16) 0.121 Uiso 0.5 1 d D U P . .
O1 O 0.22146(12) 0.1078(4) -0.50697(17) 0.080 Uiso 0.5 1 d D U P . .
H1A H 0.2299(3) 0.000000 -0.5255(4) 0.120 Uiso 1 2 d DS U P . .
H1B H 0.27070(17) 0.1637(4) -0.4551(6) 0.120 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
C6 Pd01 C6 89.4(3) . 6_565 ?
C6 Pd01 C5 178.4(2) 6_565 6_565 ?
C6 Pd01 C5 90.6(2) . 6_565 ?
C6 Pd01 C5 90.6(2) 6_565 . ?
C6 Pd01 C5 178.4(2) . . ?
C5 Pd01 C5 89.4(3) 6_565 . ?
N5 Fe2 N5 90.7(3) 5_655 6 ?
N5 Fe2 N5 180.0 5_655 . ?
N5 Fe2 N5 180.0(3) 6 2_655 ?
N5 Fe2 N5 90.7(3) 2_655 . ?
N5 Fe2 N5 89.3(3) 6 . ?
N5 Fe2 N5 89.3(3) 5_655 2_655 ?
N5 Fe2 N6 91.5(2) 5_655 . ?
N5 Fe2 N6 88.5(2) 2_655 5_655 ?
N5 Fe2 N6 91.5(2) . 5_655 ?
N5 Fe2 N6 91.5(2) 2_655 . ?
N5 Fe2 N6 88.5(2) . . ?
N5 Fe2 N6 91.5(2) 6 5_655 ?
N5 Fe2 N6 88.5(2) 6 . ?
N5 Fe2 N6 88.5(2) 5_655 5_655 ?
N6 Fe2 N6 180.0 5_655 . ?
N4 Fe1 N4 180.0 6_575 2_656 ?
N4 Fe1 N4 89.2(3) 5_676 2_656 ?
N4 Fe1 N4 89.2(3) 6_575 . ?
N4 Fe1 N4 90.8(3) 2_656 . ?
N4 Fe1 N4 180.0 5_676 . ?
N4 Fe1 N4 90.8(3) 5_676 6_575 ?
N4 Fe1 N1 89.8(2) . . ?
N4 Fe1 N1 90.2(2) 2_656 . ?
N4 Fe1 N1 89.8(2) 5_676 5_676 ?
N4 Fe1 N1 89.8(2) 6_575 . ?
N4 Fe1 N1 89.8(2) 2_656 5_676 ?
N4 Fe1 N1 90.2(2) . 5_676 ?
N4 Fe1 N1 90.2(2) 6_575 5_676 ?
N4 Fe1 N1 90.2(2) 5_676 . ?
N1 Fe1 N1 180.0 5_676 . ?
C5 N4 Fe1 175.4(5) . . ?
C6 N5 Fe2 169.5(5) . . ?
C10 N6 Fe2 120.6(7) . . ?
C7 N6 Fe2 121.9(6) . . ?
C7 N6 C10 117.5(9) . . ?
N5 C6 Pd01 176.6(6) . . ?
C1 N1 Fe1 123.6(6) . . ?
C1 N1 C4 116.5(9) . . ?
C4 N1 Fe1 119.9(7) . . ?
N4 C5 Pd01 178.4(6) . . ?
C9 N7 C10 117.6(10) . . ?
H3A N3 H3B 112.89(2) . . ?
C2 N3 H3A 120.7(4) . . ?
C2 N3 H3B 126.4(4) . . ?
N3 C2 C1 122.7(8) . . ?
N3 C2 C3 122.3(9) . . ?
C1 C2 C3 115.0(10) . . ?
C3 N2 C4 117.6(10) . . ?
N6 C10 N7 124.0(10) . . ?
N6 C10 H10 118.0 . . ?
N7 C10 H10 118.0 . . ?
N1 C1 C2 123.9(9) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C9 C8 C7 115.1(10) . . ?
N8 C8 C9 122.2(9) . . ?
N8 C8 C7 122.8(10) . . ?
N7 C9 C8 122.8(10) . . ?
N7 C9 H9 118.6 . . ?
C8 C9 H9 118.6 . . ?
N6 C7 C8 123.0(9) . . ?
N6 C7 H7 118.5 . . ?
C8 C7 H7 118.5 . . ?
N1 C4 H4 117.6 . . ?
N2 C4 N1 124.9(10) . . ?
N2 C4 H4 117.6 . . ?
C2 C3 H3 119.0 . . ?
N2 C3 C2 122.0(11) . . ?
N2 C3 H3 119.0 . . ?
C8 N8 H8A 115.8(5) . . ?
C8 N8 H8A 115.8(5) . 6 ?
C8 N8 H8B 96.3(5) . 6 ?
C8 N8 H8B 96.3(5) . . ?
H8A N8 H8A 62.6(6) . 6 ?
H8A N8 H8B 146.5(5) . 6 ?
H8A N8 H8B 112.89(2) 6 6 ?
H8A N8 H8B 112.89(2) . . ?
H8B N8 H8A 146.5(5) . 6 ?
H8B N8 H8B 50.7(8) . 6 ?
O1 O1 H1A 28.1(4) 6 . ?
O1 O1 H1B 117.2(3) 6 . ?
H1A O1 H1B 107.328(19) . . ?
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
Pd01 C6 1.973(6) . ?
Pd01 C6 1.973(6) 6_565 ?
Pd01 C5 1.978(6) 6_565 ?
Pd01 C5 1.978(6) . ?
Fe2 N5 2.142(5) 5_655 ?
Fe2 N5 2.142(5) 2_655 ?
Fe2 N5 2.142(5) . ?
Fe2 N5 2.142(5) 6 ?
Fe2 N6 2.230(8) 5_655 ?
Fe2 N6 2.230(8) . ?
Fe1 N4 2.146(5) 5_676 ?
Fe1 N4 2.146(5) 6_575 ?
Fe1 N4 2.146(5) . ?
Fe1 N4 2.146(5) 2_656 ?
Fe1 N1 2.211(8) 5_676 ?
Fe1 N1 2.211(8) . ?
N4 C5 1.150(8) . ?
N5 C6 1.154(8) . ?
N6 C10 1.339(12) . ?
N6 C7 1.295(12) . ?
N1 C1 1.309(12) . ?
N1 C4 1.351(12) . ?
N7 C10 1.351(13) . ?
N7 C9 1.299(16) . ?
N3 H3A 0.90000(15) . ?
N3 H3B 0.90000(15) . ?
N3 C2 1.323(11) . ?
C2 C1 1.399(14) . ?
C2 C3 1.406(15) . ?
N2 C4 1.343(15) . ?
N2 C3 1.327(16) . ?
C10 H10 0.9300 . ?
C1 H1 0.9300 . ?
C8 C9 1.390(16) . ?
C8 C7 1.401(14) . ?
C8 N8 1.335(11) . ?
C9 H9 0.9300 . ?
C7 H7 0.9300 . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?
N8 H8A 0.90004(14) 6 ?
N8 H8A 0.90000(14) . ?
N8 H8B 0.90005(13) 6 ?
N8 H8B 0.90000(14) . ?
O1 O1 1.589(6) 6 ?
O1 H1A 0.90000(14) . ?
O1 H1B 0.90000(13) . ?
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
Fe2 N6 C10 N7 180.000(1) . . . . ?
Fe2 N6 C7 C8 180.000(1) . . . . ?
Fe1 N1 C1 C2 180.000(2) . . . . ?
Fe1 N1 C4 N2 180.000(2) . . . . ?
N3 C2 C1 N1 180.000(2) . . . . ?
N3 C2 C3 N2 180.000(2) . . . . ?
C10 N6 C7 C8 0.000(2) . . . . ?
C10 N7 C9 C8 0.000(2) . . . . ?
C1 N1 C4 N2 0.000(4) . . . . ?
C1 C2 C3 N2 0.000(3) . . . . ?
C9 N7 C10 N6 0.000(1) . . . . ?
C9 C8 C7 N6 0.000(2) . . . . ?
C7 N6 C10 N7 0.000(1) . . . . ?
C7 C8 C9 N7 0.000(2) . . . . ?
C4 N1 C1 C2 0.000(3) . . . . ?
C4 N2 C3 C2 0.000(3) . . . . ?
C3 C2 C1 N1 0.000(2) . . . . ?
C3 N2 C4 N1 0.000(4) . . . . ?
N8 C8 C9 N7 180.000(2) . . . . ?
N8 C8 C7 N6 180.000(2) . . . . ?
