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_7046368
_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         'C19 H15 N3 O'
_chemical_formula_sum            'C19 H15 N3 O'
_chemical_formula_weight         301.34
_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   geom
_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
_cell_angle_beta                 90.073(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.3414(14)
_cell_length_b                   4.5797(2)
_cell_length_c                   12.1699(7)
_cell_measurement_reflns_used    4454
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.6040
_cell_measurement_theta_min      3.8460
_cell_volume                     1468.12(13)
_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 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.955
_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    -17.00 102.00   1.00    7.00    --   21.74  77.00-120.00  119
  2  \w    -18.00 103.00   1.00    7.00    --   21.74  77.00 120.00  121
  3  \w    -18.00 100.00   1.00    7.00    --   21.74  77.00   0.00  118
  4  \w   -115.00 -35.00   1.00    7.00    --  -20.41-178.00 -90.00   80
  5  \w    -54.00  60.00   1.00    7.00    --   21.74 -57.00-120.00  114
  6  \w    -60.00  71.00   1.00    7.00    --   21.74 -38.00  90.00  131
  7  \w    -28.00  28.00   1.00    7.00    --   21.74  91.00  43.00   56
  8  \w    -16.00  98.00   1.00    7.00    --   21.74  57.00-150.00  114
  9  \w     34.00 117.00   1.00    7.00    --   21.74-178.00 -90.00   83
 10  \w    -16.00  98.00   1.00    7.00    --   21.74  57.00 120.00  114
 11  \w    -60.00   5.00   1.00    7.00    --   21.74 -38.00 -30.00   65
 12  \w    -16.00  98.00   1.00    7.00    --   21.74  57.00  30.00  114
;
_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      0.0238483000
_diffrn_orient_matrix_UB_12      0.0652717000
_diffrn_orient_matrix_UB_13      -0.0112544000
_diffrn_orient_matrix_UB_21      -0.0057636000
_diffrn_orient_matrix_UB_22      0.0001022000
_diffrn_orient_matrix_UB_23      -0.0569346000
_diffrn_orient_matrix_UB_31      -0.0110851000
_diffrn_orient_matrix_UB_32      0.1404943000
_diffrn_orient_matrix_UB_33      0.0052409000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21498
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.434
_diffrn_reflns_theta_min         3.435
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95406
_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 orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.1117
_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^)+(0.0959P)^2^+8.0664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3051
_refine_ls_wR_factor_ref         0.3201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1910
_reflns_number_total             2538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00590g2.cif
_cod_data_source_block           l1
_cod_depositor_comments
'Adding full bibliography for 7046366--7046370.cif.'
_cod_database_code               7046368
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C19H15N3O
_reflns_odcompleteness_completeness 99.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9954(7)
 0.0046(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
3. Shared sites
{N3, C20}
{C7, N4}
4. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(N4)
Uanis(N3) = Uanis(C20)
5. Others
 Sof(H1)=Sof(O2)=Sof(H2A)=Sof(C20)=Sof(H20)=Sof(N4)=1-FVAR(1)
 Sof(H15)=Sof(O1)=Sof(H1A)=Sof(N3)=Sof(C7)=Sof(H7)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C7(H7), C20(H20)
6.b Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O2(H2A)
;
_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 1.050
_oxdiff_exptl_absorpt_empirical_full_min 0.933
_publcif_funding_html
;
;