Dual-supramolecular contacts induce extreme Hofmann framework distortion and multi-stepped spin-crossover.
Ahmed, Manan; Brand, Helen E. A.; Peterson, Vanessa K.; Clegg, Jack K.; Kepert, Cameron J.; Price, Jason R.; Powell, Benjamin J.; Neville, Suzanne M.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 1434–1442; doi:10.1039/d0dt04007j

data_7706372
_publ_section_title
;
 Dual-supramolecular contacts induce extreme Hofmann framework distortion
 and multi-stepped spin-crossover.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1434
_journal_page_last               1442
_journal_paper_doi               10.1039/d0dt04007j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C78 H54 Fe3 N42 O12 Pd3, 6(H2 O)'
_chemical_formula_sum            'C78 H66 Fe3 N42 O18 Pd3'
_chemical_formula_weight         2366.44
_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             2020-10-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-12-17 deposited with the CCDC.	2021-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                110.114(4)
_cell_angle_beta                 107.329(4)
_cell_angle_gamma                93.312(5)
_cell_formula_units_Z            1
_cell_length_a                   10.3089(12)
_cell_length_b                   15.7917(19)
_cell_length_c                   16.1627(18)
_cell_measurement_reflns_used    4494
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.5693
_cell_measurement_theta_min      2.3439
_cell_volume                     2320.6(5)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10288
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.581
_diffrn_reflns_theta_min         2.103
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.116
_exptl_absorpt_correction_T_max  0.22
_exptl_absorpt_correction_T_min  0.1574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS - Bruker- v2018.1.0'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   0.745553
_exptl_transmission_factor_min   0.649037
_refine_diff_density_max         1.756
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         10288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0923P)^2^+11.1333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.1995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6718
_reflns_number_total             10288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04007j2.cif
_cod_data_source_block           tri_150
_cod_depositor_comments
'Adding full bibliography for 7706372--7706374.cif.'
_cod_database_code               7706372
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.745553
_shelx_estimated_absorpt_t_min   0.649037
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O9A(0.5)
3.a Free rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C5(H5), C16(H16), C28(H28), C20(H20), C29(H29), C12(H12),
 C30(H30), C19(H19), C6(H6), C27(H27), C24(H24), C18(H18), C31(H31), C9(H9),
 C7(H7), C22(H22), C10(H10), C37(H37), C23(H23), C35(H35), C17(H17), C36(H36),
 C11(H11), C25(H25), C34(H34)
;
_shelx_res_checksum              54776
_olex2_submission_special_instructions 'No special instructions were received'