Direct crystallographic evidence of the reversible photo-formation and thermo-rupture of a coordination bond inducing spin-crossover phenomenon
Aguila, David; Dechambenoit, Pierre; Rouzieres, Mathieu; Mathoniere, Corine; Clerac, Rodolphe; Chem. Commun.  (2017) –; doi:10.1039/C7CC06215J

data_7120744
_publ_section_title
;
 Direct crystallographic evidence of the reversible photo-formation and
 thermo-rupture of a coordination bond inducing spin-crossover phenomenon
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06215J
_journal_year                    2017
_chemical_formula_moiety         '2(C17 H23 Fe N7), 2(C H4 O)'
_chemical_formula_sum            'C36 H54 Fe2 N14 O2'
_chemical_formula_weight         826.63
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-09 deposited with the CCDC.
2017-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.751(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8708(8)
_cell_length_b                   23.2716(18)
_cell_length_c                   15.6275(14)
_cell_measurement_reflns_used    2582
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      23.92
_cell_measurement_theta_min      2.57
_cell_volume                     3939.9(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker APEX2, intrinsic phasing'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II Quasar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29945
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.260
_diffrn_reflns_theta_min         1.573
_diffrn_source                   'Incoatec microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       plate
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.579
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         7095
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.0866
_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^)+(0.1641P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2340
_refine_ls_wR_factor_ref         0.2836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3782
_reflns_number_total             7095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06215j2.cif
_cod_data_source_block           shelx_CCDC2
_cod_database_code               7120744
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              73919