#------------------------------------------------------------------------------
#$Date: 2019-11-17 07:54:34 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228759 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/94/1549482.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_1549482
loop_
_publ_author_name
'Zenere, Katrina A.'
'Duyker, Samuel G.'
'Trzop, Elzbieta'
'Collet, Eric'
'Chan, Bun'
'Doheny, Patrick W.'
'Kepert, Cameron J.'
'Neville, Suzanne M.'
_publ_section_title
;
 Increasing spin crossover cooperativity in 2D Hofmann-type materials with
 guest molecule removal.
;
_journal_issue                   25
_journal_name_full               'Chemical science'
_journal_page_first              5623
_journal_page_last               5629
_journal_paper_doi               10.1039/c8sc01040d
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C26 H20 Fe N12 Pd, 2(O)'
_chemical_formula_sum            'C26 H20 Fe N12 O2 Pd'
_chemical_formula_weight         694.79
_chemical_melting_point          ?
_chemical_name_common            '[Fe(proptrz)2Pd(CN)4].2H2O'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-11-28 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                96.424(4)
_cell_angle_beta                 97.878(4)
_cell_angle_gamma                90.090(4)
_cell_formula_units_Z            2
_cell_length_a                   7.0836(3)
_cell_length_b                   15.1242(6)
_cell_length_c                   13.5688(6)
_cell_measurement_reflns_used    5228
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.4890
_cell_measurement_theta_min      5.9070
_cell_volume                     1430.70(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013), Xseed'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0662
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11871
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.999
_diffrn_reflns_theta_min         3.309
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.539
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
 Analytical numeric absorption correction using a multifaceted crystal
 model based on expressions derived by R.C. Clark & J.S. Reid.
 (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             688
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_recrystallization_method 'solvent diffusion'
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.436
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0331
_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)+(0.0556P)²+1.2121P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4888
_reflns_number_total             5555
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8sc01040d2.cif
_cod_data_source_block           1-Pd-2H2O-110K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1549481--1549483.cif.
;
_cod_database_code               1549482
_title
;
Guest-Modulated Room Temperature Spin Crossover with Wide Hysteresis in a
2-D Hofmann-Type Material
;
_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.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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 0.49999(3) 0.74240(2) 0.49954(2) 0.01317(9) Uani 1 1 d . . . . .
Fe1 Fe 0.0000 0.5000 0.5000 0.01059(13) Uani 1 2 d S . P . .
Fe2 Fe 1.0000 1.0000 0.5000 0.01177(14) Uani 1 2 d S . P . .
N5 N 0.0547(3) 0.51666(15) 0.64951(18) 0.0165(5) Uani 1 1 d . . . . .
N3 N 0.7899(4) 0.90002(16) 0.50147(19) 0.0167(5) Uani 1 1 d . . . . .
N6 N 0.0491(4) 0.44914(16) 0.7094(2) 0.0224(5) Uani 1 1 d . . . . .
N10 N 0.9587(4) 1.04986(17) 0.2755(2) 0.0245(5) Uani 1 1 d . . . . .
N12 N 0.8086(4) 0.86946(18) 0.0950(2) 0.0261(6) Uani 1 1 d . . . . .
N7 N 0.1277(4) 0.57384(16) 0.80436(19) 0.0211(5) Uani 1 1 d . . . . .
N8 N 0.1810(4) 0.62792(18) 0.8944(2) 0.0255(6) Uani 1 1 d . . . . .
N11 N 0.8636(4) 0.92600(17) 0.18356(19) 0.0215(5) Uani 1 1 d . . . . .
N9 N 0.9349(4) 0.98542(16) 0.33780(19) 0.0189(5) Uani 1 1 d . . . . .
N1 N 0.1904(4) 0.40613(16) 0.49749(18) 0.0149(5) Uani 1 1 d . . . . .
N4 N 0.8001(4) 1.10552(16) 0.50478(19) 0.0178(5) Uani 1 1 d . . . . .
N2 N 0.1948(4) 0.59089(15) 0.49644(18) 0.0142(5) Uani 1 1 d . . . . .
C10 C 0.3287(4) 0.9044(2) 1.1158(2) 0.0228(6) Uani 1 1 d . . . . .
C18 C 0.8144(5) 0.7870(2) 0.1054(3) 0.0279(7) Uani 1 1 d . . . . .
H18 H 0.8556 0.7686 0.1694 0.033 Uiso 1 1 calc R U . . .
C13 C 0.4409(5) 1.0469(2) 1.2605(2) 0.0288(7) Uani 1 1 d . . . . .
H13 H 0.4807 1.0953 1.3098 0.035 Uiso 1 1 calc R U . . .
C21 C 0.6679(5) 0.5868(2) -0.1167(2) 0.0238(6) Uani 1 1 d . . . . .
C1 C 0.2989(4) 0.35139(18) 0.4989(2) 0.0153(5) Uani 1 1 d . . . . .
C6 C 0.0934(5) 0.4850(2) 0.8013(2) 0.0246(6) Uani 1 1 d . . . . .
H6 H 0.1007 0.4535 0.8584 0.029 Uiso 1 1 calc R U . . .
C17 C 0.9142(5) 1.0126(2) 0.1843(2) 0.0252(6) Uani 1 1 d . . . . .
H17 H 0.9168 1.0419 0.1261 0.030 Uiso 1 1 calc R U . . .
C25 C 0.5738(5) 0.5248(2) -0.2879(2) 0.0283(7) Uani 1 1 d . . . . .
H25 H 0.5453 0.5324 -0.3569 0.034 Uiso 1 1 calc R U . . .
C20 C 0.7188(5) 0.6608(2) -0.0423(2) 0.0265(7) Uani 1 1 d . . . . .
C14 C 0.4171(5) 0.9634(2) 1.2886(2) 0.0283(7) Uani 1 1 d . . . . .
H14 H 0.4398 0.9548 1.3575 0.034 Uiso 1 1 calc R U . . .
C7 C 0.1788(5) 0.7111(2) 0.8874(2) 0.0279(7) Uani 1 1 d . . . . .
H7 H 0.1416 0.7318 0.8242 0.033 Uiso 1 1 calc R U . . .
C12 C 0.4068(5) 1.0606(2) 1.1600(3) 0.0300(7) Uani 1 1 d . . . . .
H12 H 0.4218 1.1184 1.1407 0.036 Uiso 1 1 calc R U . . .
C19 C 0.7599(5) 0.7221(2) 0.0222(3) 0.0282(7) Uani 1 1 d . . . . .
C22 C 0.6572(5) 0.5017(2) -0.0869(2) 0.0280(7) Uani 1 1 d . . . . .
H22 H 0.6858 0.4936 -0.0181 0.034 Uiso 1 1 calc R U . . .
C4 C 0.6953(4) 1.16339(18) 0.5020(2) 0.0163(6) Uani 1 1 d . . . . .
C11 C 0.3508(5) 0.9896(2) 1.0881(2) 0.0266(7) Uani 1 1 d . . . . .
H11 H 0.3273 0.9990 1.0194 0.032 Uiso 1 1 calc R U . . .
C9 C 0.2752(5) 0.8324(2) 1.0393(2) 0.0273(7) Uani 1 1 d . . . . .
C2 C 0.3047(4) 0.64668(19) 0.4985(2) 0.0149(5) Uani 1 1 d . . . . .
C5 C 0.1018(4) 0.59048(19) 0.7067(2) 0.0199(6) Uani 1 1 d . . . . .
H5 H 0.1159 0.6470 0.6841 0.024 Uiso 1 1 calc R U . . .
C3 C 0.6882(4) 0.83972(19) 0.5002(2) 0.0159(6) Uani 1 1 d . . . . .
C24 C 0.5626(5) 0.4409(2) -0.2574(2) 0.0307(7) Uani 1 1 d . . . . .
H24 H 0.5256 0.3912 -0.3055 0.037 Uiso 1 1 calc R U . . .
C8 C 0.2316(5) 0.7735(2) 0.9736(2) 0.0271(7) Uani 1 1 d . . . . .
C26 C 0.6266(5) 0.5981(2) -0.2182(2) 0.0271(7) Uani 1 1 d . . . . .
H26 H 0.6346 0.6556 -0.2394 0.033 Uiso 1 1 calc R U . . .
C16 C 0.8776(4) 0.9120(2) 0.2812(2) 0.0219(6) Uani 1 1 d . . . . .
H16 H 0.8502 0.8572 0.3049 0.026 Uiso 1 1 calc R U . . .
C23 C 0.6052(5) 0.4292(2) -0.1571(3) 0.0302(7) Uani 1 1 d . . . . .
H23 H 0.5986 0.3714 -0.1364 0.036 Uiso 1 1 calc R U . . .
C15 C 0.3604(5) 0.8916(2) 1.2176(2) 0.0257(7) Uani 1 1 d . . . . .
H15 H 0.3432 0.8342 1.2376 0.031 Uiso 1 1 calc R U . . .
O1WA O 0.0167(10) 0.2669(3) 0.6760(4) 0.0281(7) Uiso 0.529(9) 1 d . U P A 1
O1WB O -0.0522(11) 0.2690(3) 0.6950(4) 0.0281(7) Uiso 0.471(9) 1 d . U P A 2
O2WA O 1.0881(8) 1.2280(3) 0.2984(3) 0.0299(8) Uiso 0.607(7) 1 d . U P B 3
O2WB O 1.0139(12) 1.2285(4) 0.3199(5) 0.0299(8) Uiso 0.393(7) 1 d . U P B 4
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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
C3 Pd1 C4 86.20(11) . 2_676
C3 Pd1 C2 178.46(10) . .
C4 Pd1 C2 92.26(11) 2_676 .
C3 Pd1 C1 92.81(11) . 2_666
C4 Pd1 C1 179.01(10) 2_676 2_666
C2 Pd1 C1 88.72(11) . 2_666
N2 Fe1 N2 180.0 2_566 .
N2 Fe1 N1 91.13(10) 2_566 2_566
N2 Fe1 N1 88.87(10) . 2_566
N2 Fe1 N1 88.87(10) 2_566 .
N2 Fe1 N1 91.13(10) . .
N1 Fe1 N1 180.0 2_566 .
N2 Fe1 N5 88.68(10) 2_566 2_566
N2 Fe1 N5 91.32(10) . 2_566
N1 Fe1 N5 89.33(10) 2_566 2_566
N1 Fe1 N5 90.67(10) . 2_566
N2 Fe1 N5 91.32(10) 2_566 .
N2 Fe1 N5 88.68(10) . .
N1 Fe1 N5 90.67(10) 2_566 .
N1 Fe1 N5 89.33(10) . .
N5 Fe1 N5 180.0 2_566 .
N3 Fe2 N3 180.0 . 2_776
N3 Fe2 N4 86.48(9) . 2_776
N3 Fe2 N4 93.53(9) 2_776 2_776
N3 Fe2 N4 93.52(9) . .
N3 Fe2 N4 86.47(9) 2_776 .
N4 Fe2 N4 180.0 2_776 .
N3 Fe2 N9 88.08(9) . .
N3 Fe2 N9 91.92(9) 2_776 .
N4 Fe2 N9 91.61(9) 2_776 .
N4 Fe2 N9 88.39(9) . .
N3 Fe2 N9 91.92(9) . 2_776
N3 Fe2 N9 88.08(9) 2_776 2_776
N4 Fe2 N9 88.39(9) 2_776 2_776
N4 Fe2 N9 91.61(9) . 2_776
N9 Fe2 N9 180.0 . 2_776
C5 N5 N6 108.4(2) . .
C5 N5 Fe1 127.3(2) . .
N6 N5 Fe1 124.32(18) . .
C3 N3 Fe2 173.5(3) . .
C6 N6 N5 106.7(2) . .
C17 N10 N9 106.7(2) . .
C18 N12 N11 114.6(3) . .
C6 N7 C5 105.1(2) . .
C6 N7 N8 122.1(3) . .
C5 N7 N8 132.8(3) . .
C7 N8 N7 115.0(3) . .
C17 N11 C16 105.4(3) . .
C17 N11 N12 122.9(3) . .
C16 N11 N12 131.7(3) . .
C16 N9 N10 107.7(3) . .
C16 N9 Fe2 125.7(2) . .
N10 N9 Fe2 126.44(19) . .
C1 N1 Fe1 177.8(3) . .
C4 N4 Fe2 176.0(3) . .
C2 N2 Fe1 176.3(3) . .
C11 C10 C15 119.4(3) . .
C11 C10 C9 118.9(3) . .
C15 C10 C9 121.8(3) . .
N12 C18 C19 120.7(3) . .
N12 C18 H18 119.7 . .
C19 C18 H18 119.7 . .
C14 C13 C12 120.2(3) . .
C14 C13 H13 119.9 . .
C12 C13 H13 119.9 . .
C22 C21 C26 119.4(3) . .
C22 C21 C20 119.2(3) . .
C26 C21 C20 121.4(3) . .
N1 C1 Pd1 177.6(3) . 2_666
N6 C6 N7 110.6(3) . .
N6 C6 H6 124.7 . .
N7 C6 H6 124.7 . .
N10 C17 N11 110.6(3) . .
N10 C17 H17 124.7 . .
N11 C17 H17 124.7 . .
C24 C25 C26 120.4(3) . .
C24 C25 H25 119.8 . .
C26 C25 H25 119.8 . .
C19 C20 C21 178.4(4) . .
C13 C14 C15 120.8(3) . .
C13 C14 H14 119.6 . .
C15 C14 H14 119.6 . .
N8 C7 C8 120.6(3) . .
N8 C7 H7 119.7 . .
C8 C7 H7 119.7 . .
C11 C12 C13 119.7(3) . .
C11 C12 H12 120.1 . .
C13 C12 H12 120.1 . .
C20 C19 C18 173.6(4) . .
C23 C22 C21 120.4(3) . .
C23 C22 H22 119.8 . .
C21 C22 H22 119.8 . .
N4 C4 Pd1 175.8(3) . 2_676
C12 C11 C10 120.4(3) . .
C12 C11 H11 119.8 . .
C10 C11 H11 119.8 . .
C8 C9 C10 178.4(4) . .
N2 C2 Pd1 178.6(3) . .
N5 C5 N7 109.2(3) . .
N5 C5 H5 125.4 . .
N7 C5 H5 125.4 . .
N3 C3 Pd1 176.0(3) . .
C23 C24 C25 120.2(3) . .
C23 C24 H24 119.9 . .
C25 C24 H24 119.9 . .
C9 C8 C7 173.3(4) . .
C25 C26 C21 119.7(3) . .
C25 C26 H26 120.2 . .
C21 C26 H26 120.2 . .
N9 C16 N11 109.5(3) . .
N9 C16 H16 125.3 . .
N11 C16 H16 125.3 . .
C22 C23 C24 120.0(3) . .
C22 C23 H23 120.0 . .
C24 C23 H23 120.0 . .
C14 C15 C10 119.4(3) . .
C14 C15 H15 120.3 . .
C10 C15 H15 120.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C3 1.983(3) .
Pd1 C4 1.987(3) 2_676
Pd1 C2 1.998(3) .
Pd1 C1 2.012(3) 2_666
Fe1 N2 1.955(3) 2_566
Fe1 N2 1.955(3) .
Fe1 N1 1.961(2) 2_566
Fe1 N1 1.961(2) .
Fe1 N5 2.000(2) 2_566
Fe1 N5 2.000(2) .
Fe2 N3 2.124(3) .
Fe2 N3 2.124(3) 2_776
Fe2 N4 2.137(3) 2_776
Fe2 N4 2.137(3) .
Fe2 N9 2.172(3) .
Fe2 N9 2.172(3) 2_776
N5 C5 1.302(4) .
N5 N6 1.378(3) .
N3 C3 1.158(4) .
N6 C6 1.299(4) .
N10 C17 1.298(4) .
N10 N9 1.384(3) .
N12 C18 1.270(4) .
N12 N11 1.403(4) .
N7 C6 1.361(4) .
N7 C5 1.364(4) .
N7 N8 1.398(3) .
N8 C7 1.272(4) .
N11 C17 1.355(4) .
N11 C16 1.355(4) .
N9 C16 1.308(4) .
N1 C1 1.130(4) .
N4 C4 1.149(4) .
N2 C2 1.143(4) .
C10 C11 1.397(5) .
C10 C15 1.403(4) .
C10 C9 1.430(4) .
C18 C19 1.421(4) .
C18 H18 0.9500 .
C13 C14 1.376(5) .
C13 C12 1.391(5) .
C13 H13 0.9500 .
C21 C22 1.396(5) .
C21 C26 1.398(4) .
C21 C20 1.432(4) .
C1 Pd1 2.012(3) 2_666
C6 H6 0.9500 .
C17 H17 0.9500 .
C25 C24 1.384(5) .
C25 C26 1.390(5) .
C25 H25 0.9500 .
C20 C19 1.207(5) .
C14 C15 1.389(5) .
C14 H14 0.9500 .
C7 C8 1.424(4) .
C7 H7 0.9500 .
C12 C11 1.385(5) .
C12 H12 0.9500 .
C22 C23 1.383(5) .
C22 H22 0.9500 .
C4 Pd1 1.987(3) 2_676
C11 H11 0.9500 .
C9 C8 1.197(5) .
C5 H5 0.9500 .
C24 C23 1.385(5) .
C24 H24 0.9500 .
C26 H26 0.9500 .
C16 H16 0.9500 .
C23 H23 0.9500 .
C15 H15 0.9500 .
