Near-Infrared Photoswitching of Azobenzenes under Physiological Conditions.
Dong, Mingxin; Babalhavaeji, Amirhossein; Collins, Catherine V.; Jarrah, Kareem; Sadovski, Oleg; Dai, Qiuyun; Woolley, G. Andrew; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b06471

data_4126423
_publ_section_title
;
 Near-Infrared Photoswitching of Azobenzenes under Physiological
 Conditions.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b06471
_journal_year                    2017
_chemical_formula_moiety         'C18 H16 Br2 N2 O6, 2(C H Cl3)'
_chemical_formula_sum            'C20 H18 Br2 Cl6 N2 O6'
_chemical_formula_weight         754.88
_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
_audit_creation_date             2016-04-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.652(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8792(4)
_cell_length_b                   15.5118(5)
_cell_length_c                   8.0195(3)
_cell_measurement_reflns_used    1652
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.3810
_cell_measurement_theta_min      5.0200
_cell_volume                     1325.45(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41k (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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_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    -96.00 -58.00   1.00    1.00    --  -41.49 125.00  30.00   38
  2  \w   -110.00 -24.00   1.00    1.00    --  -41.49 -37.00 150.00   86
  3  \w   -110.00 -21.00   1.00    1.00    --  -41.49 -37.00-120.00   89
  4  \w     25.00 100.00   1.00    1.00    --  107.19 -94.00 -30.00   75
  5  \w     90.00 131.00   1.00    1.00    --  107.19 -45.00  60.00   41
  6  \w     79.00 130.00   1.00    1.00    --  107.19 -30.00  30.00   51
  7  \w     80.00 168.00   1.00    1.00    --  107.19  30.00-120.00   88
  8  \w    142.00 178.00   1.00    1.00    --  107.19 125.00  30.00   36
  9  \w     37.00 120.00   1.00    1.00    --  107.19 -61.00 -30.00   83
 10  \w     36.00  73.00   1.00    1.00    --  107.19 -45.00  60.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1328785000
_diffrn_orient_matrix_UB_12      0.0116483000
_diffrn_orient_matrix_UB_13      -0.1087352000
_diffrn_orient_matrix_UB_21      -0.0565366000
_diffrn_orient_matrix_UB_22      -0.0161643000
_diffrn_orient_matrix_UB_23      0.1586641000
_diffrn_orient_matrix_UB_31      0.0064176000
_diffrn_orient_matrix_UB_32      0.0972404000
_diffrn_orient_matrix_UB_33      0.0392116000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4813
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.096
_diffrn_reflns_theta_min         4.149
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.811
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41k (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.304
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0609P)^2^+1.0201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2130
_reflns_number_total             2590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06471_si_003.cif
_cod_data_source_block           20160428b
_cod_original_cell_volume        1325.44(8)
_cod_database_code               4126423
_chemical_oxdiff_formula         c1h1n1o1Br1
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              55034
_shelx_hkl_checksum              96734
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-28
_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 1.573
_oxdiff_exptl_absorpt_empirical_full_min 0.650