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_7715898
_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
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-21 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                94.756(5)
_cell_angle_beta                 94.062(5)
_cell_angle_gamma                115.990(6)
_cell_formula_units_Z            2
_cell_length_a                   9.1702(6)
_cell_length_b                   10.3930(6)
_cell_length_c                   15.0356(10)
_cell_measurement_reflns_used    5183
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      29.7870
_cell_measurement_theta_min      2.4690
_cell_volume                     1274.41(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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     -9.00  74.00   0.50   10.00    --   11.27  63.00 171.00  166
  2  \w    -63.00  34.00   0.50   10.00    --   11.27 -63.00  35.00  194
  3  \w     -3.00  28.00   0.50   10.00    --  -11.03 -99.00-120.00   62
  4  \w    -42.00  56.00   0.50   10.00    --  -11.03  77.00-150.00  196
  5  \w    -22.00  26.00   0.50   10.00    --  -11.03 -99.00  90.00   96
  6  \w    -64.00   4.00   0.50   10.00    --   11.27 -19.00  60.00  136
  7  \w    -17.00  35.50   0.50   10.00    --   11.27 -99.00 -30.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0670834000
_diffrn_orient_matrix_UB_12      0.0697972000
_diffrn_orient_matrix_UB_13      0.0081127000
_diffrn_orient_matrix_UB_21      -0.0371675000
_diffrn_orient_matrix_UB_22      0.0232501000
_diffrn_orient_matrix_UB_23      -0.0339498000
_diffrn_orient_matrix_UB_31      -0.0403818000
_diffrn_orient_matrix_UB_32      0.0211496000
_diffrn_orient_matrix_UB_33      0.0324805000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7027
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.437
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense brown'
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.942
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         7027
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0679P)^2^+3.4670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6419
_reflns_number_total             7027
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9623\% 
around [-0.00 0.00 1.00] (reciprocal) or [0.21 0.20 0.96] (direct)
;
_cod_data_source_file            d4dt00870g2.cif
_cod_data_source_block           shs_78_gaal_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7715897--7715901.cif.'
_cod_original_cell_volume        1274.41(15)
_cod_database_code               7715898
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H30N12FePd1
_chemical_oxdiff_usercomment     M2Pd(compusil1)
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.734
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4881(12)
 0.5119(12)
2. 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
3. Restrained distances
 C23-C23X
 0.56 with sigma of 0.001
 C23X-C24 = C24-C23
 1.5 with sigma of 0.01
 C23X-C24 \\sim C24-C23
 with sigma of 0.01
 N11-C23 \\sim N11X-C23X
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(N11) = Uanis(N11X)
Uanis(C23) = Uanis(C23X)
5. Others
 Sof(N11)=Sof(C23)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(N11X)=Sof(C23X)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
6.a Riding coordinates:
 C24(H24A,H24B,H24C,H24D,H24E,H24F), O2W(H2WA,H2WB), O1W(H1WA,H1WB)
6.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)
;
_shelx_res_checksum              83291
_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 1.551
_oxdiff_exptl_absorpt_empirical_full_min 0.684
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2