Tunable Conjugated Organoborane Oligomers for Visible-Light-Driven Hydrogen Evolution
Ru, Chenglong; Wei, Qiuyu; Chen, Wenhao; Guan, Qiye; Zhang, Qianqian; Ling, Yuan; Tao, Chunlan; Qin, Dongdong; Wu, Jincai; Pan, Xiaobo; ACS Energy Letters 5 (2020) 669–675; doi:10.1021/acsenergylett.0c00075

data_4517388
_publ_section_title
;
 Tunable Conjugated Organoborane Oligomers for Visible-Light-Driven
 Hydrogen Evolution
;
_journal_issue                   2
_journal_name_full               'ACS Energy Letters'
_journal_page_first              669
_journal_page_last               675
_journal_paper_doi               10.1021/acsenergylett.0c00075
_journal_volume                  5
_journal_year                    2020
_chemical_formula_moiety         'C27 H29 B Br2'
_chemical_formula_sum            'C27 H29 B Br2'
_chemical_formula_weight         524.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                73.946(10)
_cell_angle_beta                 88.380(8)
_cell_angle_gamma                77.430(9)
_cell_formula_units_Z            2
_cell_length_a                   9.1165(8)
_cell_length_b                   10.8798(13)
_cell_length_c                   13.0957(15)
_cell_measurement_reflns_used    2506
_cell_measurement_temperature    181(13)
_cell_measurement_theta_max      26.4470
_cell_measurement_theta_min      3.8120
_cell_volume                     1217.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      181(13)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega -105.00  -57.00   1.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1983 -178.0000  120.0000 32

  2 omega  -17.00   28.00   1.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1983  -99.0000    0.0000 30

  3 omega   -3.00   97.50   1.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0108   57.0000  150.0000 67

  4 omega   35.00   62.00   1.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0108  178.0000  -60.0000 18

  5 omega   74.00  113.00   1.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0108  178.0000  -60.0000 26

  6 omega  -44.00   43.00   1.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0108  -57.0000  -90.0000 58

  7 omega    6.00  105.00   1.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0108   38.0000   60.0000 66
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0061324000
_diffrn_orient_matrix_UB_12      0.0457667000
_diffrn_orient_matrix_UB_13      0.0302054000
_diffrn_orient_matrix_UB_21      0.0478733000
_diffrn_orient_matrix_UB_22      -0.0477692000
_diffrn_orient_matrix_UB_23      0.0404352000
_diffrn_orient_matrix_UB_31      0.0635005000
_diffrn_orient_matrix_UB_32      0.0213610000
_diffrn_orient_matrix_UB_33      -0.0251569000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7927
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.239
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.340
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'yellow green'
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0252P)^2^+0.5262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3649
_reflns_number_total             4799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nz0c00075_si_002.cif
_cod_data_source_block           ruchl_0516
_cod_depositor_comments
;Adding full bibliography for 4517388.cif.

 Adding full bibliography for 4517388.cif.
;
_cod_database_code               4517388
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22), C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C15(H15), C17(H17)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              47563
_shelx_hkl_checksum              79051
_olex2_date_sample_data_collection 2018-05-16
_olex2_submission_special_instructions 'No special instructions were received'