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_7123296
_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), H2 O, C14 H16 N2'
_chemical_formula_sum            'C14 H18 Br2 N2 O'
_chemical_formula_weight         390.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-04
_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                90
_cell_angle_beta                 114.868(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6558(11)
_cell_length_b                   11.4656(3)
_cell_length_c                   6.9238(3)
_cell_measurement_reflns_used    11646
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.3800
_cell_measurement_theta_min      2.0680
_cell_volume                     1487.73(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.15a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 512
_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     -5.76 200.24   0.50   10.00    --   31.63  73.80 -70.76  412
  2  \w     -5.76 200.24   0.50   10.00    --   31.63  73.80 154.24  412
  3  \w     -5.76 200.24   0.50   10.00    --   31.63  73.80-160.76  412
  4  \w     -5.76 200.24   0.50   10.00    --   31.63  73.80 109.24  412
  5  \w     -2.76 200.24   0.50   10.00    --   31.63  73.80-115.76  406
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0171646000
_diffrn_orient_matrix_UB_12      -0.0225880000
_diffrn_orient_matrix_UB_13      0.0617235000
_diffrn_orient_matrix_UB_21      0.0177342000
_diffrn_orient_matrix_UB_22      0.0419674000
_diffrn_orient_matrix_UB_23      0.0802665000
_diffrn_orient_matrix_UB_31      -0.0286943000
_diffrn_orient_matrix_UB_32      0.0394474000
_diffrn_orient_matrix_UB_33      -0.0499799000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16543
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.500
_diffrn_reflns_theta_min         2.082
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.443
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15a (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    1.742
_exptl_crystal_description       needle
_exptl_crystal_F_000             776
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.087
_exptl_crystal_size_rad          0.2
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         2261
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+5.6455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1887
_reflns_number_total             2261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01150a2.cif
_cod_data_source_block           mk-5-23-2016
_cod_database_code               7123296
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C56  H68  Br8  N8  O4  '
_shelx_estimated_absorpt_t_max   0.649
_shelx_estimated_absorpt_t_min   0.414
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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,H) groups
2. Restrained distances
 H1_$1-O1 = O1-H1
 0.975 with sigma of 0.02
 H1_$1-H1
 1.568 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C2, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C3, C4
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 C4, C7
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 C4, C5
 with sigma for 1-2 distances of 0.0003 and sigma for 1-3 distances of 0.0003
 C5, C6
 with sigma for 1-2 distances of 0.0003 and sigma for 1-3 distances of 0.0003
 C6, N1
 with sigma for 1-2 distances of 0.0003 and sigma for 1-3 distances of 0.0003
 N1, C2
 with sigma for 1-2 distances of 0.0003 and sigma for 1-3 distances of 0.0003
 C1, C1
 with sigma for 1-2 distances of 0.0003 and sigma for 1-3 distances of 0.0003
 C1, N1
 with sigma for 1-2 distances of 0.0003 and sigma for 1-3 distances of 0.0003
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C2(H2), C3(H3)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              41529
_shelx_hkl_checksum              37935
_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 DQ42
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.297
_oxdiff_exptl_absorpt_empirical_full_min 0.770