Amino group promoted photocatalytic hydrogen evolution activity observed in two copper(ii)-based layered complexes.
Li, Lei; Zhu, Shuang; Hao, Rui; Wang, Jia-Jun; Yang, En-Cui; Zhao, Xiao-Jun; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12726–12733; doi:10.1039/c8dt02803f

data_7047267
_publ_section_title
;
 Amino group promoted photocatalytic hydrogen evolution activity observed
 in two copper(ii)-based layered complexes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12726
_journal_page_last               12733
_journal_paper_doi               10.1039/c8dt02803f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C50 H35 Cu N7 O6'
_chemical_formula_sum            'C50 H35 Cu N7 O6'
_chemical_formula_weight         893.39
_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             2017-10-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-03 deposited with the CCDC.
2018-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                82.193(6)
_cell_angle_beta                 87.050(6)
_cell_angle_gamma                72.875(6)
_cell_formula_units_Z            1
_cell_length_a                   7.1100(5)
_cell_length_b                   10.9172(8)
_cell_length_c                   13.7599(10)
_cell_measurement_reflns_used    1663
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.2410
_cell_measurement_theta_min      4.2690
_cell_volume                     1011.17(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -69.00  32.00   1.00    2.32    --  -41.24  57.00   0.00  101
  2  \w   -113.00 -13.00   1.00    2.32    --  -41.24 -57.00-150.00  100
  3  \w    -96.00  -2.00   1.00    2.32    --  -41.24 125.00  30.00   94
  4  \w   -116.00 -17.00   1.00    2.32    --  -41.24 -38.00  90.00   99
  5  \w     34.00 121.00   1.00    9.28    --  107.08-125.00-180.00   87
  6  \w     34.00 121.00   1.00    9.28    --  107.08-125.00   0.00   87
  7  \w     81.00 178.00   1.00    9.28    --  107.08  45.00 -60.00   97
  8  \w     25.00 109.00   1.00    9.28    --  107.08 -95.00-150.00   84
  9  \w     78.00 178.00   1.00    9.28    --  107.08  61.00-180.00  100
 10  \w     94.00 178.00   1.00    9.28    --  107.08 125.00 120.00   84
 11  \w     37.00  80.00   1.00    9.28    --  107.08 -30.00 -30.00   43
 12  \w    108.00 135.00   1.00    9.28    --  107.08 -30.00 -30.00   27
 13  \w     37.00  88.00   1.00    9.28    --  107.08 -45.00-180.00   51
 14  \w     85.00 145.00   1.00    9.28    --  107.08  77.00  60.00   60
 15  \w     94.00 127.00   1.00    9.28    --  107.08 125.00   0.00   33
 16  \w     49.00 140.00   1.00    9.28    --  107.08 -77.00 -30.00   91
;
_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      -0.1153001000
_diffrn_orient_matrix_UB_12      -0.0202661000
_diffrn_orient_matrix_UB_13      0.0957520000
_diffrn_orient_matrix_UB_21      0.0635103000
_diffrn_orient_matrix_UB_22      0.1062081000
_diffrn_orient_matrix_UB_23      0.0407283000
_diffrn_orient_matrix_UB_31      -0.1846239000
_diffrn_orient_matrix_UB_32      0.1023088000
_diffrn_orient_matrix_UB_33      -0.0441062000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2331
_diffrn_reflns_av_unetI/netI     0.2909
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7041
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.071
_diffrn_reflns_theta_max         67.071
_diffrn_reflns_theta_min         4.272
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.288
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.467
_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         1.842
_refine_diff_density_min         -2.015
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3601
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.2252
_refine_ls_R_factor_gt           0.1637
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3632
_refine_ls_wR_factor_ref         0.4191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1711
_reflns_number_total             3601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02803f2.cif
_cod_data_source_block           a170813b
_cod_depositor_comments
'Adding full bibliography for 7047267--7047268.cif.'
_cod_original_cell_volume        1011.16(13)
_cod_database_code               7047267
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
Uanis(C22) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C22) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3. Others
 Fixed Sof: H24(0.5) N4(0.5) H4A(0.5) H4B(0.5)
4.a Rotating group:
 N4(H4A,H4B)
4.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)
4.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_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 4.390
_oxdiff_exptl_absorpt_empirical_full_min 0.255