Optimizing Electron Transfer from CdSe QDs to Hydrogenase for Photocatalytic H2 Production
Sanchez, Monica Kiewit; Wu, Chang-hao; Adams, Michael W.; Dyer, Richard Brian; Chemical Communications  (2019) –; doi:10.1039/C9CC01150A

data_7123294
_publ_section_title
;
 Optimizing Electron Transfer from CdSe QDs to Hydrogenase for
 Photocatalytic H2 Production
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01150A
_journal_year                    2019
_chemical_formula_moiety         '2(Br), C H4 O, C14 H16 N2'
_chemical_formula_sum            'C15 H20 Br2 N2 O'
_chemical_formula_weight         404.15
_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             2019-02-08
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2019-02-08 deposited with the CCDC.    2019-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                104.745(2)
_cell_angle_beta                 96.597(2)
_cell_angle_gamma                103.047(3)
_cell_formula_units_Z            2
_cell_length_a                   7.3138(2)
_cell_length_b                   10.0105(3)
_cell_length_c                   12.1578(2)
_cell_measurement_reflns_used    8364
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.8750
_cell_measurement_theta_min      3.8070
_cell_volume                     824.44(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.953
_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     82.00 119.00   0.50    1.00    --  105.75-125.00-120.00   74
  2  \w     86.00 117.00   0.50    1.00    --  105.75-125.00  90.00   62
  3  \w     62.00 106.00   0.50    1.00    --  105.75-125.00  60.00   88
  4  \w     35.00  73.00   0.50    1.00    --  105.75-125.00  90.00   76
  5  \w     39.00  74.00   0.50    1.00    --  105.75-125.00-120.00   70
  6  \w   -104.00 -70.00   0.50    0.25    --  -49.66-125.00 -60.00   68
  7  \w   -120.00 -73.00   0.50    0.25    --  -49.66-125.00  60.00   94
  8  \w     81.00 107.00   0.50    1.00    --  105.75 -95.00 -60.00   52
  9  \w     65.00 108.00   0.50    1.00    --  105.75 -95.00 150.00   86
 10  \w     35.00  61.00   0.50    1.00    --  105.75 -95.00 -60.00   52
 11  \w     38.00  76.00   0.50    1.00    --  105.75 -77.00  60.00   76
 12  \w     69.00 100.00   0.50    1.00    --  105.75 -77.00 120.00   62
 13  \w     38.00  88.00   0.50    1.00    --  105.75 -77.00  90.00  100
 14  \w     35.00  62.00   0.50    1.00    --  105.75 -77.00 120.00   54
 15  \w     52.00  77.00   0.50    1.00    --  105.75 -45.00 -60.00   50
 16  \w     34.00  83.00   0.50    1.00    --  105.75 -45.00 -30.00   98
 17  \w     34.00  84.00   0.50    1.00    --  105.75 -45.00-180.00  100
 18  \w     37.00  64.00   0.50    1.00    --  105.75 -28.00  98.00   54
 19  \w     11.00  37.00   0.50    0.25    --   49.66 -28.00  98.00   52
 20  \w   -111.00 -45.00   0.50    0.25    --  -49.66 -28.00  98.00  132
 21  \w   -158.00 -81.00   0.50    1.00    --  -84.25 -28.00  98.00  154
 22  \w    -20.00  54.00   0.50    0.25    --   49.66 -19.00 -60.00  148
 23  \w     98.00 178.00   0.50    1.00    --  105.75  28.00 -99.00  160
 24  \w     68.00 118.00   0.50    0.25    --   49.66  28.00 -99.00  100
 25  \w    -10.00  19.00   0.50    0.25    --  -49.66  28.00 -99.00   58
 26  \w    -56.00 -15.00   0.50    0.25    --  -49.66  28.00 -99.00   82
 27  \w    -70.00 -37.00   0.50    1.00    --  -84.25  28.00 -99.00   66
 28  \w    102.00 176.00   0.50    1.00    --  105.75  30.00 -30.00  148
 29  \w     99.00 176.00   0.50    1.00    --  105.75  30.00   0.00  154
 30  \w    137.00 175.00   0.50    1.00    --  105.75 125.00  60.00   76
 31  \w    150.00 175.00   0.50    1.00    --  105.75 125.00  30.00   50
 32  \w    106.00 139.00   0.50    1.00    --  105.75 125.00  30.00   66
 33  \w     94.00 126.00   0.50    1.00    --  105.75 125.00  60.00   64
 34  \w    -58.00 -25.00   0.50    1.00    --  -84.25 125.00   0.00   66
 35  \w    -91.00 -35.00   0.50    1.00    --  -84.25 125.00 -90.00  112
 36  \w    -91.00 -64.00   0.50    1.00    --  -84.25 125.00   0.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1684762000
_diffrn_orient_matrix_UB_12      -0.0470997000
_diffrn_orient_matrix_UB_13      -0.0483181000
_diffrn_orient_matrix_UB_21      -0.0904463000
_diffrn_orient_matrix_UB_22      -0.1547328000
_diffrn_orient_matrix_UB_23      -0.0000758000
_diffrn_orient_matrix_UB_31      -0.1086510000
_diffrn_orient_matrix_UB_32      -0.0329092000
_diffrn_orient_matrix_UB_33      -0.1242112000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9300
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.039
_diffrn_reflns_theta_min         3.824
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.213
_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.183
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.0033(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3321
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0453P)^2^+0.7799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3210
_reflns_number_total             3321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01150a2.cif
_cod_data_source_block           dq52
_cod_database_code               7123294
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30  H40  Br4  N4  O2  '
_shelx_estimated_absorpt_t_max   0.396
_shelx_estimated_absorpt_t_min   0.295
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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, All C(H,H,H,H) groups
2. Restrained distances
 O1-H1
 0.955 with sigma of 0.005
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C7(H7), C10(H10), C5(H5), C12(H12)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              78563
_shelx_hkl_checksum              18784
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id DQ52
_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 1.670
_oxdiff_exptl_absorpt_empirical_full_min 0.742