A biomimetic self-assembly Cobaloxime@CdS/rGO hybrid for boosting photocatalytic H2 production
Wang, Feng; Hu, Jun-Chao; Sun, Shanshan; Li, Ming-De; Xia, Wu; Wu, Jin; Liu, Hongfang; Chemical Communications  (2019) –; doi:10.1039/C9CC08512B

data_7124456
_publ_section_title
;
 A biomimetic self-assembly Cobaloxime@CdS/rGO hybrid for boosting
 photocatalytic H2 production
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC08512B
_journal_year                    2019
_chemical_formula_moiety
'C34 H36 Cl Co N6 O5, 0.5(C H Cl3), 0.5(H2 O)'
_chemical_formula_sum            'C34.5 H37.5 Cl2.5 Co N6 O5.5'
_chemical_formula_weight         771.76
_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
_audit_creation_date             2019-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-05 deposited with the CCDC.	2019-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                95.311(2)
_cell_angle_beta                 91.077(2)
_cell_angle_gamma                95.834(2)
_cell_formula_units_Z            4
_cell_length_a                   8.8077(6)
_cell_length_b                   14.2501(11)
_cell_length_c                   28.349(2)
_cell_measurement_reflns_used    3157
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.39
_cell_measurement_theta_min      2.33
_cell_volume                     3523.0(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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(2)
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.1200
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            25133
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        23.995
_diffrn_reflns_theta_max         23.995
_diffrn_reflns_theta_min         1.443
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Bruker,2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     907
_refine_ls_number_reflns         10443
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1515
_refine_ls_R_factor_gt           0.0704
_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^)+(0.0945P)^2^+1.7962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.2019
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5469
_reflns_number_total             10443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08512b2.cif
_cod_data_source_block           mo_191030b_0m
_cod_original_formula_sum        'C34.50 H37.50 Cl2.50 Co N6 O5.50'
_cod_database_code               7124456
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.958
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C28-C23 = C23-C22 = C31-C22 = C31-C30 = C30-C29
 1.39 with sigma of 0.01
 C22-C21 = C21-C20 = C20-C19 = C24-C19 = C28-C23 = C24-C23 = C25-C24 = C26-C25
 = C27-C26
 1.39 with sigma of 0.01
 O4-H4 = O4A-H4AD = O2A-H2A = O2-H2
 0.95 with sigma of 0.02
 H2A-N2A
 2 with sigma of 0.04
 H4AD-N4A = H4-N4 = H2-N2
 2 with sigma of 0.04
 H4AD-O1A
 1.6 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C29) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C22)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19A) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C26A) \\sim Ueq,
Uanis(C27A) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C33A) \\sim Ueq,
Uanis(C29A) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C31A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl2) \\sim Ueq, Uanis(Cl0A) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(Cl3)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Free rotating group:
 O5(H5D,H5E)
4.b Ternary CH refined with riding coordinates:
 C0AA(H0AA)
4.c Secondary CH2 refined with riding coordinates:
 C14A(H14C,H14D), C16A(H16C,H16D), C17A(H17C,H17D), C18A(H18C,H18D), C14(H14A,
 H14B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B)
4.d Aromatic/amide H refined with riding coordinates:
 C9A(H9A), C10A(H10A), C12A(H12A), C13A(H13A), C20A(H20A), C21A(H21A),
 C25A(H25A), C26A(H26A), C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A),
 C34A(H34A), N6A(H6A), C9(H9), C10(H10), C12(H12), C13(H13), C20(H20), C21(H21),
  C25(H25), C26(H26), C34(H34), C33(H33), C32(H32), C31(H31), C30(H30), N6(H6)
4.e Fitted hexagon refined as free rotating group:
 C27(C34,C33,C32,C29,C28)
4.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,
 H5AC), C8A(H8AA,H8AB,H8AC), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C)
;
_olex2_submission_special_instructions 'No special instructions were received'