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_7046366
_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         'C38 H28 Cl Fe N6 O2, H2 O'
_chemical_formula_sum            'C38 H30 Cl Fe N6 O3'
_chemical_formula_weight         709.98
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-04-19 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.83(14)
_cell_angle_beta                 115.38(9)
_cell_angle_gamma                92.78(15)
_cell_formula_units_Z            2
_cell_length_a                   11.917(9)
_cell_length_b                   12.08(3)
_cell_length_c                   13.350(12)
_cell_measurement_reflns_used    128
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5470
_cell_measurement_theta_min      6.3860
_cell_volume                     1733(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -10.00  99.00   1.00    7.50    --   24.65  57.00  60.00  109
  2  \w    -24.00 104.00   1.00    7.50    --   24.65  38.00  60.00  128
  3  \w    -10.00  99.00   1.00    7.50    --   24.65  57.00 -90.00  109
  4  \w    -68.00  53.00   1.00    7.50    --  -27.22  77.00 150.00  121
  5  \w    -20.00  26.00   1.00    7.50    --  -27.22 -99.00-120.00   46
  6  \w    -20.00  26.00   1.00    7.50    --  -27.22 -99.00  30.00   46
  7  \w   -101.00   7.00   1.00    7.50    --  -27.22 -57.00 120.00  108
  8  \w    -49.00  59.00   1.00    7.50    --   24.65 -57.00 120.00  108
  9  \w     35.00 115.00   1.00    7.50    --   24.65 178.00 -30.00   80
 10  \w    -55.00  73.00   1.00    7.50    --   24.65 -38.00  30.00  128
 11  \w    -49.00  59.00   1.00    7.50    --   24.65 -57.00   0.00  108
 12  \w    -20.00  26.00   1.00    7.50    --  -27.22 -99.00 150.00   46
 13  \w   -101.00   7.00   1.00    7.50    --  -27.22 -57.00  90.00  108
 14  \w   -118.00 -35.00   1.00    7.50    --  -27.22-178.00-150.00   83
 15  \w    -56.00  65.00   1.00    7.50    --   24.65 -77.00  30.00  121
 16  \w     34.00 116.00   1.00    7.50    --   24.65-178.00-150.00   82
 17  \w    -63.00 112.00   1.00    7.50    --   24.65   0.00-180.00  175
 18  \w    -63.00 112.00   1.00    7.50    --   24.65   0.00-150.00  175
 19  \w    -63.00 112.00   1.00    7.50    --   24.65   0.00-120.00  175
 20  \w    -63.00 112.00   1.00    7.50    --   24.65   0.00 -90.00  175
 21  \w     45.00 109.00   1.00    7.50    --   24.65 166.00  28.00   64
 22  \w    -63.00 112.00   1.00    7.50    --   24.65   0.00 -30.00  175
 23  \w    -63.00 112.00   1.00    7.50    --   24.65   0.00   0.00  175
 24  \w    -63.00  93.00   1.00    7.50    --   24.65   0.00  30.00  156
;
_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      0.0281273000
_diffrn_orient_matrix_UB_12      -0.0182292000
_diffrn_orient_matrix_UB_13      0.0551052000
_diffrn_orient_matrix_UB_21      0.0314428000
_diffrn_orient_matrix_UB_22      0.0529662000
_diffrn_orient_matrix_UB_23      0.0184482000
_diffrn_orient_matrix_UB_31      -0.0508308000
_diffrn_orient_matrix_UB_32      0.0179886000
_diffrn_orient_matrix_UB_33      0.0091691000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1228
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            66525
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.689
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95501
_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    1.360
_exptl_crystal_description       plate
_exptl_crystal_F_000             734
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.223
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0667
_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^)+(0.1077P)^2^+1.0387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.2049
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3963
_reflns_number_total             6103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00590g2.cif
_cod_data_source_block           Fe(L1-H)2Cl
_cod_depositor_comments
'Adding full bibliography for 7046366--7046370.cif.'
_cod_original_cell_volume        1733(4)
_cod_database_code               7046366
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2. Others
 Sof(O2B)=Sof(H2BA)=Sof(H2BB)=Sof(O2C)=Sof(H2CA)=Sof(H2CB)=0.5*(1-FVAR(2))
 Sof(O2A)=Sof(H2AA)=Sof(H2AB)=FVAR(1)
3.a Riding coordinates:
 O2A(H2AA,H2AB), O2B(H2BA,H2BB), O2C(H2CA,H2CB)
3.b Aromatic/amide H refined with riding coordinates:
 C7'(H7'), C9(H9), C10(H10), C12(H12), C2(H2), C13(H13), C7(H7), C13'(H13'),
 C5'(H5'), C9'(H9'), C12'(H12'), C2'(H2'), C10'(H10'), C3(H3), C5(H5), C4'(H4'),
  C15'(H15'), C19'(H19'), C15(H15), C18'(H18'), C4(H4), C3'(H3'), C19(H19),
 C17'(H17'), C16'(H16'), C16(H16), C18(H18), C17(H17)
;
_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 1.116
_oxdiff_exptl_absorpt_empirical_full_min 0.948
_publcif_funding_html
;
;