Substituent group-tunable hydrogen evolution activity observed in isostructural Cu(ii)-based coordination polymer photocatalysts.
Dai, Xue-Jiao; Wang, Jia-Jun; Li, Lei; Ding, Bo; Liu, Zheng-Yu; Zhao, Xiao-Jun; Yang, En-Cui; Dalton transactions (Cambridge, England : 2003) 49 (2020) 1674–1680; doi:10.1039/c9dt04567h

data_7703054
_publ_section_title
;
 Substituent group-tunable hydrogen evolution activity observed in
 isostructural Cu(ii)-based coordination polymer photocatalysts.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1674
_journal_page_last               1680
_journal_paper_doi               10.1039/c9dt04567h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C50 H30 Br Cu N6 O6, 2(H)'
_chemical_formula_sum            'C50 H32 Br Cu N6 O6'
_chemical_formula_weight         956.26
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-05 deposited with the CCDC.	2019-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                82.290(4)
_cell_angle_beta                 87.182(4)
_cell_angle_gamma                72.275(4)
_cell_formula_units_Z            1
_cell_length_a                   7.2467(13)
_cell_length_b                   10.935(2)
_cell_length_c                   13.919(3)
_cell_measurement_temperature    296(2)
_cell_volume                     1041.1(3)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0961
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6040
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.971
_exptl_absorpt_coefficient_mu    1.545
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0915 before and 0.0387 after correction.
The Ratio of minimum to maximum transmission is 0.8690.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.576
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         3663
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1339
_refine_ls_R_factor_gt           0.0911
_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^)+(0.1103P)^2^+4.3466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2312
_refine_ls_wR_factor_ref         0.2565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2466
_reflns_number_total             3663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04567h2.cif
_cod_data_source_block           n180327a
_cod_depositor_comments
'Adding full bibliography for 7703052--7703054.cif.'
_cod_database_code               7703054
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.768
_shelx_estimated_absorpt_t_min   0.727
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, H of C23, HA of C23'
 At 1.2 times of:
  H14 of C14, H21 of C21, H10 of C10, H9 of C9, H8 of C8, H25 of C25, H25' of
  C25', H17 of C17, H18 of C18, H15 of C15, H13 of C13, H12 of C12, H7 of C7,
  H5 of C5, H2 of C2
2. Restrained distances
 C23-Br1
 1.65 with sigma of 0.01
 C23-C24 = C24-C25
 1.38 with sigma of 0.01
 C23-C25
 2.37 with sigma of 0.01
 C23'-Br1'
 1.65 with sigma of 0.01
 C23'-C24 = C24-C25'
 1.38 with sigma of 0.01
 C23'-C25'
 2.37 with sigma of 0.01
3. Restrained planarity
 C23, C24, C25, Br1, C22
 with sigma of 0.001
 C23', C24, C25', Br1', C22
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(Br1) = Uanis(Br1')
Uanis(C25) = Uanis(C25')
Uanis(C23) = Uanis(C23')
5. Others
 Fixed Sof: Br1(0.4) C25(0.8) H25(0.8) C23(0.8) H(0.8) Br1'(0.1) C25'(0.2)
 H25'(0.2) C23'(0.2) HA(0.2)
6.a Riding coordinates:
 O3(H3), C23(H), C23'(HA)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C21(H21), C25(H25), C25'(H25')
;
_shelx_res_checksum              22452
_olex2_submission_special_instructions 'No special instructions were received'