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_7703052
_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 H34 Cu N6 O7'
_chemical_formula_sum            'C50 H34 Cu N6 O7'
_chemical_formula_weight         894.37
_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     dual
_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                81.707(4)
_cell_angle_beta                 88.055(4)
_cell_angle_gamma                72.596(4)
_cell_formula_units_Z            1
_cell_length_a                   7.1213(3)
_cell_length_b                   10.9493(5)
_cell_length_c                   13.8046(6)
_cell_measurement_reflns_used    3515
_cell_measurement_temperature    139.1(3)
_cell_measurement_theta_max      73.8150
_cell_measurement_theta_min      3.2050
_cell_volume                     1016.32(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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      139.1(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -116.00  -9.00   1.00    1.57    --  -41.24 -19.00 120.00  107
  2  \w   -116.00 -40.00   1.00    1.57    --  -41.24 -38.00  60.00   76
  3  \w    -81.00 -11.00   1.00    1.57    --  -41.24 125.00-150.00   70
  4  \w     24.00  55.00   1.00    1.57    --   41.24-125.00  30.00   31
  5  \w     29.00  91.00   1.00    1.57    --   41.24-125.00 120.00   62
  6  \w     84.00 164.00   1.00    6.26    --  107.08  45.00  30.00   80
  7  \w     81.00 121.00   1.00    6.26    --  107.08  45.00-150.00   40
  8  \w     79.00 139.00   1.00    6.26    --  107.08 -77.00 -60.00   60
  9  \w     37.00 121.00   1.00    6.26    --  107.08-125.00 -30.00   84
 10  \w     55.00 173.00   1.00    6.26    --  107.08  15.00 -30.00  118
 11  \w     51.00  83.00   1.00    6.26    --  107.08 -30.00  30.00   32
 12  \w     92.00 135.00   1.00    6.26    --  107.08 -30.00  30.00   43
 13  \w    131.00 176.00   1.00    6.26    --  107.08  77.00-150.00   45
 14  \w     40.00  80.00   1.00    6.26    --  107.08 -61.00 -60.00   40
 15  \w     90.00 116.00   1.00    6.26    --  107.08  77.00-150.00   26
 16  \w     68.00 120.00   1.00    6.26    --  107.08-125.00 150.00   52
 17  \w     33.00 140.00   1.00    6.26    --  107.08 -77.00 120.00  107
 18  \w     33.00  60.00   1.00    6.26    --  107.08 -77.00 -60.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.2194838000
_diffrn_orient_matrix_UB_12      0.0073586000
_diffrn_orient_matrix_UB_13      0.0051621000
_diffrn_orient_matrix_UB_21      -0.0047069000
_diffrn_orient_matrix_UB_22      0.0013441000
_diffrn_orient_matrix_UB_23      -0.1116445000
_diffrn_orient_matrix_UB_31      0.0566322000
_diffrn_orient_matrix_UB_32      -0.1487407000
_diffrn_orient_matrix_UB_33      0.0151224000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6457
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.063
_diffrn_reflns_theta_max         67.063
_diffrn_reflns_theta_min         3.235
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             461
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3633
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0573P)^2^+0.3012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3137
_reflns_number_total             3633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04567h2.cif
_cod_data_source_block           a180427c
_cod_depositor_comments
'Adding full bibliography for 7703052--7703054.cif.'
_cod_original_cell_volume        1016.33(8)
_cod_database_code               7703052
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.782
_shelx_estimated_absorpt_t_min   0.738
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O4-C24
 1.42 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: H24(0.5) O4(0.5) H4(0.5)
5.a Riding coordinates:
 O4(H4)
5.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), C20(H20), C21(H21), C24(H24), C25(H25)
5.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              11407
_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 4.411
_oxdiff_exptl_absorpt_empirical_full_min 0.632