Spin State Chemistry: Modulation of Ligand p K<sub>a</sub> by Spin State Switching in a [2× 2] Iron(II) Grid-Type Complex.
Dhers, Sébastien; Mondal, Abhishake; Aguilà, David; Ramírez, Juan; Vela, Sergi; Dechambenoit, Pierre; Rouzières, Mathieu; Nitschke, Jonathan R.; Clérac, Rodolphe; Lehn, Jean-Marie; Journal of the American Chemical Society 140 (2018) 8218–8227; doi:10.1021/jacs.8b03735

data_4132412
_publ_section_title
;
 Spin State Chemistry: Modulation of Ligand p K<sub>a</sub> by Spin State
 Switching in a [2\\times 2] Iron(II) Grid-Type Complex.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8218
_journal_page_last               8227
_journal_paper_doi               10.1021/jacs.8b03735
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C88 H72 N32 Zn4, 8(B F4), 3(C2 H3 N)'
_chemical_formula_sum            'C94 H81 B8 F32 N35 Zn4'
_chemical_formula_weight         2656.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 110.798(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5838(5)
_cell_length_b                   35.6460(10)
_cell_length_c                   18.5501(5)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.31
_cell_measurement_theta_min      2.71
_cell_volume                     12105.7(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            119103
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.864
_diffrn_reflns_theta_min         2.413
_diffrn_source                   'Cu-ImuS microfocus tube'
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       prism
_exptl_crystal_F_000             5352
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;
The residual electron density was assigned to five molecules of the acetonitrile solvent [459/4= 115 e per asymmetric unit; five molecules of C2H3N1 would give 110 e]. 
;
_refine_diff_density_max         1.289
_refine_diff_density_min         -2.149
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1429
_refine_ls_number_reflns         21271
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1458
_refine_ls_R_factor_gt           0.1211
_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^)+(0.0337P)^2^+180.8675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2573
_refine_ls_wR_factor_ref         0.2674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15658
_reflns_number_total             21271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b03735_si_007.cif
_cod_data_source_block           jmlsd170807
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4132412
_shelx_estimated_absorpt_t_min   0.556
_shelx_estimated_absorpt_t_max   0.809
_shelxl_version_number           2013-4
_shelx_res_checksum              12700
_shelx_hkl_checksum              23390