New cyanido-bridged iron(II) spin crossover coordination polymers with an unusual ladder-like topology: an alternative to Hofmann clathrates.
Visinescu, Diana; Shylin, Sergii I.; Shova, Sergiu; Novitchi, Ghenadie; Popescu, Delia-Laura; Alexandru, Maria-Gabriela; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9062–9071; doi:10.1039/d4dt00870g

data_7715899
_publ_section_title
;
 New cyanido-bridged iron(II) spin crossover coordination polymers with an
 unusual ladder-like topology: an alternative to Hofmann clathrates.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9062
_journal_page_last               9071
_journal_paper_doi               10.1039/d4dt00870g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H25 Fe N12, 2(C2 N2 Pd0.5), 3.167(H2 O)'
_chemical_formula_sum            'C40 H31.33 Fe N16 O3.17 Pd'
_chemical_formula_weight         949.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-09
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-03-21 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                101.995(7)
_cell_angle_beta                 93.012(7)
_cell_angle_gamma                102.090(6)
_cell_formula_units_Z            2
_cell_length_a                   9.8400(8)
_cell_length_b                   11.7209(9)
_cell_length_c                   18.2393(15)
_cell_measurement_reflns_used    3643
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.9590
_cell_measurement_theta_min      1.8430
_cell_volume                     2001.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 41.123a 64-bit (release 20-01-2022))'
_computing_data_reduction        'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -55.00 -28.00   1.00   50.00    --  -15.29 104.00-132.00   27
  2  \w    -18.00  59.00   1.00   50.00    --   17.71-104.00 126.00   77
  3  \w    -32.00  -5.00   1.00   50.00    --  -15.29  77.00   0.00   27
  4  \w    -44.00  56.00   1.00   50.00    --  -15.29  19.00 -30.00  100
  5  \w     -6.00  19.00   1.00   50.00    --  -15.29 104.00-132.00   25
  6  \w     17.00  44.00   1.00   50.00    --  -15.29  57.00 120.00   27
  7  \w    -75.00 -39.00   1.00   50.00    --  -15.29-178.00 -60.00   36
  8  \w      1.00  39.00   1.00   50.00    --   17.71  77.00-150.00   38
  9  \w     -1.00  87.00   1.00   50.00    --   17.71  38.00-120.00   88
 10  \w     -9.00  39.00   1.00   50.00    --   17.71  77.00 -30.00   48
 11  \w     40.00  68.00   1.00   50.00    --   17.71 178.00  90.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10550
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.316
_diffrn_reflns_theta_min         1.823
_exptl_absorpt_coefficient_mu    0.874
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       prism
_exptl_crystal_F_000             961
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.956
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         10550
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0628
_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/[\s^2^(Fo^2^)+(0.0778P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6822
_reflns_number_total             10550
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9012\% 
around [0.00 -0.00 1.00] (reciprocal) or [0.18 0.32 0.93] (direct)
;
_cod_data_source_file            d4dt00870g2.cif
_cod_data_source_block           shi_6031_gaal_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7715897--7715901.cif.'
_cod_database_code               7715899
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.880
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5114(11)
 0.4886(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Pd2-C41X \\sim Pd2-C41
 with sigma of 0.01
 N16-C41 \\sim N16X-C41X
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N16) \\sim Ueq, Uanis(N16X) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.02
Uanis(O5W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N16X) = Uanis(N16)
Uanis(C41) = Uanis(C41X)
5. Others
 Sof(N16)=Sof(C41)=1-FVAR(1)
 Sof(N16X)=Sof(C41X)=FVAR(1)
 Fixed Sof: O3W(0.5) H3WA(0.5) H3WB(0.5) O4W(0.33333) H4WA(0.33333)
 H4WB(0.33333) O5W(0.33333) H5WA(0.33333) H5WB(0.33333)
6.a Riding coordinates:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
6.b Free rotating group:
 O1W(H1WA,H1WB)
6.c Aromatic/amide H refined with riding coordinates:
 N4(H4), C1(H1), C2(H2), C3(H3), C4(H4A), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C28(H28), C29(H29), C30(H30), C31(H31), C34(H34), C35(H35),
 C36(H36), C37(H37)
;
_shelx_res_checksum              27573
_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
;