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_7715897
_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         'C22 H12 Fe N10 Pd, C2 H3 N, 2(H2 O)'
_chemical_formula_sum            'C24 H19 Fe N11 O2 Pd'
_chemical_formula_weight         655.75
_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             2024-01-10
_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                94.888(4)
_cell_angle_beta                 93.429(4)
_cell_angle_gamma                116.505(6)
_cell_formula_units_Z            2
_cell_length_a                   9.2277(6)
_cell_length_b                   10.5250(6)
_cell_length_c                   15.0648(6)
_cell_measurement_reflns_used    4206
_cell_measurement_temperature    180.00(14)
_cell_measurement_theta_max      29.1120
_cell_measurement_theta_min      2.1850
_cell_volume                     1296.70(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 38.46 (release 23-01-2017))'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.838
_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    -31.00  14.00   1.00   50.00    --  -15.29 -19.00  30.00   45
  2  \w    -30.00  51.00   1.00   50.00    --  -15.29  57.00   0.00   81
  3  \w     -9.00  84.00   1.00   50.00    --   17.55  77.00-150.00   93
  4  \w      1.00  55.00   1.00   50.00    --   17.55  57.00 120.00   54
  5  \w     10.00  87.00   1.00   50.00    --   17.55  38.00 -60.00   77
  6  \w     24.00  57.00   1.00   50.00    --   17.55 -99.00   0.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0580861838
_diffrn_orient_matrix_UB_12      -0.0625510310
_diffrn_orient_matrix_UB_13      0.0156696024
_diffrn_orient_matrix_UB_21      0.0586737951
_diffrn_orient_matrix_UB_22      -0.0260626774
_diffrn_orient_matrix_UB_23      0.0037432278
_diffrn_orient_matrix_UB_31      0.0255179535
_diffrn_orient_matrix_UB_32      0.0342006299
_diffrn_orient_matrix_UB_33      0.0447294793
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11197
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.184
_diffrn_reflns_theta_min         2.179
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91359
_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            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5891
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+0.9199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4898
_reflns_number_total             5891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00870g2.cif
_cod_data_source_block           shi_4406_gaal
_cod_depositor_comments
'Adding full bibliography for 7715897--7715901.cif.'
_cod_database_code               7715897
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20N8O2Fe1Pd2
_chemical_oxdiff_usercomment     M2PdFepytri
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.926
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C23X-C24 = C24-C23
 1.52 with sigma of 0.01
 N11-C23 \\sim N11X-C23X
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N11) \\sim Ueq, Uanis(N11X) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N11) = Uanis(N11X)
Uanis(C23X) = Uanis(C23)
4. Others
 Fixed Sof: N11X(0.5) N11(0.5) C23(0.5) C23X(0.5) H24D(0.5) H24E(0.5)
 H24F(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
5.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18)
5.c Idealised Me refined as rotating group:
 C24(H24D,H24E,H24F), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              67337
_olex2_date_sample_data_collection 2024-01-10
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.150
_oxdiff_exptl_absorpt_empirical_full_min 0.831