“Normal” and “reverse” spin crossover induced by two different structural events in iron(II) coordination polymer
Weselski, Marek Damian; Książek, Maria; Mess, Pamela; Kusz, Joachim; Bronisz, Robert; Chemical Communications  (2019) –; doi:10.1039/C9CC02755F

data_7123444
_publ_section_title
;
 &#x201C;Normal&#x201D; and &#x201C;reverse&#x201D; spin crossover induced
 by two different structural events in iron(II) coordination polymer
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02755F
_journal_year                    2019
_chemical_formula_moiety
;
C84 H138 Fe3 N42, 6(C F3 O3 S), 12(C2 H3 N)
;
_chemical_formula_sum            'C114 H174 F18 Fe3 N54 O18 S6'
_chemical_formula_weight         3290.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-03-25 deposited with the CCDC.    2019-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                64.830(11)
_cell_angle_beta                 74.777(11)
_cell_angle_gamma                85.360(9)
_cell_formula_units_Z            1
_cell_length_a                   12.1229(15)
_cell_length_b                   18.3542(18)
_cell_length_c                   20.670(3)
_cell_measurement_reflns_used    2965
_cell_measurement_temperature    225(1)
_cell_measurement_theta_max      23.4770
_cell_measurement_theta_min      3.3490
_cell_volume                     4014.0(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2018)'
_diffrn_ambient_temperature      225(1)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.701
_diffrn_measured_fraction_theta_max 0.701
_diffrn_measurement_device_type
;
SuperNova diffractometer (Agilent Technologies) with Atlas detector
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.701
_diffrn_reflns_Laue_measured_fraction_max 0.701
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17025
_diffrn_reflns_point_group_measured_fraction_full 0.701
_diffrn_reflns_point_group_measured_fraction_max 0.701
_diffrn_reflns_theta_full        24.558
_diffrn_reflns_theta_max         24.558
_diffrn_reflns_theta_min         3.130
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         9433
_refine_ls_number_restraints     407
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1057P)^2^+3.4150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1787
_refine_ls_wR_factor_ref         0.2225
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5854
_reflns_number_total             9433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02755f2.cif
_cod_data_source_block           9_rb18_pm30_4b_11_225k
_cod_original_cell_volume        4014.0(9)
_cod_database_code               7123444
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.917
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              82728