Iron(ii) complexes of tris(2-pyridylmethyl)amine (TPMA) and neutral bidentate ligands showing thermal- and photo-induced spin crossover.
García-López, Víctor; Waerenborgh, João C; Vieira, Bruno J. C.; Clemente-León, Miguel; Coronado, Eugenio; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9156–9163; doi:10.1039/c8dt01425f

data_7046707
_publ_section_title
;
 Iron(ii) complexes of tris(2-pyridylmethyl)amine (TPMA) and neutral
 bidentate ligands showing thermal- and photo-induced spin crossover.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9156
_journal_page_last               9163
_journal_paper_doi               10.1039/c8dt01425f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '2(Cl O4), C20 H26 Fe N6'
_chemical_formula_sum            'C20 H26 Cl2 Fe N6 O8'
_chemical_formula_weight         605.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           34
_space_group_name_Hall           'P 2 -2n'
_space_group_name_H-M_alt        'P n n 2'
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-29
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-06-14 deposited with the CCDC.
2018-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9207(6)
_cell_length_b                   15.7742(6)
_cell_length_c                   9.8061(5)
_cell_measurement_reflns_used    3505
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      21.2000
_cell_measurement_theta_min      4.0470
_cell_volume                     2617.35(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.15
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -52.00 -18.00   1.00   18.50    --  -20.96 -66.00 -70.53   34
  2  \w    -42.00   2.00   1.00   18.50    --  -20.96 -69.00 -45.98   44
  3  \w    -84.00   4.00   1.00   18.50    --  -20.96 -69.00  53.56   88
  4  \w    -35.00  -9.00   1.00   18.50    --  -20.96 -68.00  97.24   26
  5  \w    -48.00  47.00   1.00   18.50    --   21.90 -68.00 162.40   95
  6  \w    -47.00 -10.00   1.00   18.50    --   21.90 -57.00  30.00   37
  7  \w     67.00  92.00   1.00   18.50    --   21.90  69.00 -70.78   25
  8  \w    -45.00  48.00   1.00   18.50    --   21.90 -66.00 -85.41   93
  9  \w     -1.00  25.00   1.00   18.50    --   21.90  69.00 -70.78   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0865
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23100
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         3.433
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5990
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.0871
_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^)+(0.1465P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2189
_refine_ls_wR_factor_ref         0.2644
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3515
_reflns_number_total             5990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01425f2.cif
_cod_data_source_block           vg20k
_cod_depositor_comments
'Adding full bibliography for 7046707--7046711.cif.'
_cod_database_code               7046707
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.906
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.91(6)
 0.09(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
3. Restrained distances
 N2B-C6B
 1.5 with sigma of 0.02
 C20B-N6B
 1.49 with sigma of 0.02
 N5B-C19B
 1.5 with sigma of 0.02
 O5-O7A
 2.3 with sigma of 0.02
 N6B-N5B
 2.7 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C18A \\sim C14B: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04
C15A \\sim C17B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C8A \\sim C12B: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04
C9A \\sim C11B: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04
C10A \\sim C10B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C11A \\sim C9B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C12A \\sim C8B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cl2A \\sim Cl2B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
O8A \\sim O8B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O7A \\sim O7B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Fixed Sof: C1A(0.85) H1A(0.85) C2A(0.85) H2A(0.85) C3A(0.85) H3A(0.85)
 C4A(0.85) H4A(0.85) C5A(0.85) C6A(0.85) H6AA(0.85) H6AB(0.85) C7A(0.85)
 H7AA(0.85) H7AB(0.85) C8A(0.85) C9A(0.85) H9A(0.85) C10A(0.85) H10A(0.85)
 C11A(0.85) H11A(0.85) C12A(0.85) H12A(0.85) C13A(0.85) H13A(0.85) H13B(0.85)
 C14A(0.85) C15A(0.85) H15A(0.85) C16A(0.85) H16A(0.85) C17A(0.85) H17A(0.85)
 C18A(0.85) H18A(0.85) C19A(0.85) H19A(0.85) H19B(0.85) C20A(0.85) H20A(0.85)
 H20B(0.85) Fe1A(0.85) N1A(0.85) N2A(0.85) N3A(0.85) N4A(0.85) N5A(0.85)
 H5AA(0.85) H5AB(0.85) N6A(0.85) H6AC(0.85) H6AD(0.85) C1B(0.15) H1B(0.15)
 C2B(0.15) H2B(0.15) C3B(0.15) H3B(0.15) C4B(0.15) H4B(0.15) C5B(0.15)
 N1B(0.15) C6B(0.15) H6BA(0.15) H6BB(0.15) C7B(0.15) H7BA(0.15) H7BB(0.15)
 C8B(0.15) C9B(0.15) H9B(0.15) C10B(0.15) H10B(0.15) C11B(0.15) H11B(0.15)
 C12B(0.15) H12B(0.15) N3B(0.15) C13B(0.15) H13C(0.15) H13D(0.15) C14B(0.15)
 C15B(0.15) H15B(0.15) C16B(0.15) H16B(0.15) C17B(0.15) H17B(0.15) C18B(0.15)
 H18B(0.15) N4B(0.15) C19B(0.15) H19C(0.15) H19D(0.15) C20B(0.15) H20C(0.15)
 H20D(0.15) Fe1B(0.15) N2B(0.15) N5B(0.15) H5BA(0.15) H5BB(0.15) N6B(0.15)
 H6BC(0.15) H6BD(0.15) Cl2A(0.5) O7A(0.5) O8A(0.5) Cl2B(0.5) O7B(0.5) O8B(0.5)
 Fixed Uiso: C13B(0.05) C20B(0.05) N5B(0.07577)
 Fixed X: C13B(0.63904) N5B(0.69287)
 Fixed Y: C13B(0.61477) N5B(0.66695)
 Fixed Z: C13B(0.59105) N5B(0.11935)
6.a Secondary CH2 refined with riding coordinates:
 C6A(H6AA,H6AB), C7A(H7AA,H7AB), C13A(H13A,H13B), C19A(H19A,H19B), C20A(H20A,
 H20B), N5A(H5AA,H5AB), N6A(H6AC,H6AD), C6B(H6BA,H6BB), C7B(H7BA,H7BB),
 C13B(H13C,H13D), C19B(H19C,H19D), C20B(H20C,H20D), N5B(H5BA,H5BB), N6B(H6BC,
 H6BD)
6.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C9A(H9A), C10A(H10A), C11A(H11A),
 C12A(H12A), C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A), C1B(H1B), C2B(H2B),
  C3B(H3B), C4B(H4B), C9B(H9B), C10B(H10B), C11B(H11B), C12B(H12B), C15B(H15B),
 C16B(H16B), C17B(H17B), C18B(H18B)
6.c Fitted hexagon refined as free rotating group:
 C1B(C2B,C3B,C4B,C5B,N1B), C8B(C9B,C10B,C11B,C12B,N3B), C14B(C15B,C16B,C17B,
 C18B,N4B)
;
_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
;