Photoswitchable transition metal complexes with azobenzene-functionalized imine-based ligands: structural and kinetic analysis.
Markiewicz, G.; Walczak, A.; Perlitius, F.; Piasecka, M.; Harrowfield, J. M.; Stefankiewicz, A. R.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14254–14262; doi:10.1039/c8dt00590g

data_7046370
_publ_section_title
;
 Photoswitchable transition metal complexes with azobenzene-functionalized
 imine-based ligands: structural and kinetic analysis.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14254
_journal_page_last               14262
_journal_paper_doi               10.1039/c8dt00590g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C76 H56 Fe2 N12 O5'
_chemical_formula_sum            'C76 H56 Fe2 N12 O5'
_chemical_formula_weight         1329.02
_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_date             2018-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-05-07 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                80.582(5)
_cell_angle_beta                 75.100(5)
_cell_angle_gamma                76.309(5)
_cell_formula_units_Z            2
_cell_length_a                   10.5729(6)
_cell_length_b                   17.7529(12)
_cell_length_c                   18.6545(12)
_cell_measurement_reflns_used    4565
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.6610
_cell_measurement_theta_min      1.5420
_cell_volume                     3267.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0296
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     35.00 115.00   1.00    8.00    --   24.65 178.00 -30.00   80
  2  \w   -101.00   7.00   1.00    8.00    --  -27.22 -57.00-150.00  108
  3  \w   -108.00  14.00   1.00    8.00    --  -27.22 -77.00 -30.00  122
  4  \w    -62.00  47.00   1.00    8.00    --  -27.22  57.00   0.00  109
  5  \w    -20.00  26.00   1.00    8.00    --  -27.22 -99.00  60.00   46
  6  \w    -62.00  47.00   1.00    8.00    --  -27.22  57.00  90.00  109
  7  \w   -111.00  53.00   1.00    8.00    --  -27.22 -19.00   0.00  164
  8  \w   -101.00   7.00   1.00    8.00    --  -27.22 -57.00 150.00  108
  9  \w    -76.00  52.00   1.00    8.00    --  -27.22  38.00-150.00  128
 10  \w   -118.00 -34.00   1.00    8.00    --  -27.22 178.00 -30.00   84
 11  \w    -63.00 112.00   1.00    8.00    --   24.65   0.00-180.00  175
 12  \w     35.00 115.00   1.00    8.00    --   24.65 178.00-120.00   80
 13  \w    -45.00  -6.00   1.00    8.00    --   24.65 130.00 179.22   39
 14  \w    -49.00  59.00   1.00    8.00    --   24.65 -57.00  60.00  108
 15  \w    -10.00  99.00   1.00    8.00    --   24.65  57.00 -30.00  109
 16  \w    -20.00  26.00   1.00    8.00    --  -27.22 -99.00   0.00   46
 17  \w    -20.00  26.00   1.00    8.00    --  -27.22 -99.00  90.00   46
 18  \w   -116.00 -38.00   1.00    8.00    --  -27.22-176.00-162.00   78
 19  \w    -63.00 112.00   1.00    8.00    --   24.65   0.00-120.00  175
 20  \w    -63.00 112.00   1.00    8.00    --   24.65   0.00 -90.00  175
 21  \w    -63.00 112.00   1.00    8.00    --   24.65   0.00 -60.00  175
 22  \w    -63.00  54.00   1.00    8.00    --   24.65   0.00 -30.00  117
 23  \w    -63.00 112.00   1.00    8.00    --   24.65   0.00-150.00  175
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0262467000
_diffrn_orient_matrix_UB_12      -0.0166737000
_diffrn_orient_matrix_UB_13      0.0364577000
_diffrn_orient_matrix_UB_21      -0.0082410000
_diffrn_orient_matrix_UB_22      0.0361360000
_diffrn_orient_matrix_UB_23      0.0139294000
_diffrn_orient_matrix_UB_31      -0.0653609000
_diffrn_orient_matrix_UB_32      0.0113024000
_diffrn_orient_matrix_UB_33      -0.0066102000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2483
_diffrn_reflns_av_unetI/netI     0.1346
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            100798
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        23.533
_diffrn_reflns_theta_max         23.533
_diffrn_reflns_theta_min         4.110
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         9648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1519
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+1.3926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5083
_reflns_number_total             9648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00590g2.cif
_cod_data_source_block           fe2(l1-h)4o
_cod_depositor_comments
'Adding full bibliography for 7046366--7046370.cif.'
_cod_database_code               7046370
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         FeC30H60N10O6
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
N2B': within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
N3B': within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
3.a Aromatic/amide H refined with riding coordinates:
 C13A(H13A), C12A(H12A), C7A'(H7A'), C7B'(H7B'), C13B(H13B), C10A(H10A),
 C7A(H7A), C9A'(H9A'), C9A(H9A), C5A'(H5A'), C7B(H7B), C9B(H9B), C2(H2),
 C2A(H2A), C3(H3), C5A(H5A), C4(H4), C2A'(H2A'), C3A'(H3A'), C10B(H10B),
 C12B(H12B), C3A(H3A), C4A'(H4A'), C19B(H19B), C4A(H4A), C5B'(H5B'), C18B(H18B),
  C15A(H15A), C5B(H5B), C2B(H2B), C19A(H19A), C4B'(H4B'), C9B'(H9B'),
 C3B'(H3B'), C7(H7), C2B'(H2B'), C17B(H17B), C15B(H15B), C4B(H4B), C8(H8),
 C9(H9), C10(H10), C11(H11), C17A(H17A), C3B(H3B), C16A(H16A), C18A(H18A),
 C13(H13), C14(H14), C16B(H16B), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C1C(H1C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.039
_oxdiff_exptl_absorpt_empirical_full_min 0.963
_publcif_funding_html
;
;