Electrocatalytic water oxidation studies of a tetranuclear Cu(ii) complex with cubane-like core Cu4(μ3-O)4
Gao, Wei-Song; Wang, Jin-Miao; Shi, Ning-Ning; Chen, Chang-Neng; Fan, Yu-Hua; Wang, Mei; New Journal of Chemistry 43 (2019) 4640–; doi:10.1039/C8NJ06263C

data_7058201
_publ_section_title
;
 Electrocatalytic water oxidation studies of a tetranuclear Cu(ii) complex
 with cubane-like core Cu4(\m3-O)4
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4640
_journal_paper_doi               10.1039/C8NJ06263C
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C32 H38 Cu4 N4 O12, 3(H2 O), 2(N O3)'
_chemical_formula_sum            'C32 H44 Cu4 N6 O21'
_chemical_formula_weight         1102.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-16
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-16 deposited with the CCDC.    2019-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.306(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.785(3)
_cell_length_b                   17.746(3)
_cell_length_c                   16.689(3)
_cell_measurement_reflns_used    6139
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.549
_cell_measurement_theta_min      2.423
_cell_volume                     4003.4(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      173.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17767
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.553
_diffrn_reflns_theta_min         1.894
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1333 before and 0.0577 after correction. The Ratio of minimum to maximum transmission is 0.6996. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4599
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+1.4177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3891
_reflns_number_total             4599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj06263c2.cif
_cod_data_source_block           mo_2017524-2017062208_0m
_cod_depositor_comments          'Adding full bibliography for 7058201.cif.'
_cod_original_cell_volume        4003.2(13)
_cod_database_code               7058201
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.795
_shelx_estimated_absorpt_t_min   0.579
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O4-H4
 0.86 with sigma of 0.02
 O6-N4 \\sim O8-N4 \\sim O10-N4
 with sigma of 0.02
 O7-N3 \\sim O9-N3 \\sim O11-N3
 with sigma of 0.02
 O8-O6 \\sim O6-O10
 with sigma of 0.02
 O7-O9 \\sim O9-O11
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O7) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O7) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O8) \\sim
Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11)
\\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.012
4. Others
 Fixed Sof: O7(0.55) O11(0.55) N3(0.55) O9(0.55) O6(0.45) N4(0.45) O8(0.45)
 O10(0.45) O2W(0.5) H2WA(0.5) H2WB(0.5)
5.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C1(H1A,H1B), C14(H14A,H14B), C7(H7A,H7B)
5.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C3(H3), C10(H10), C5(H5), C11(H11), C4(H4A)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
;
_olex2_submission_special_instructions 'No special instructions were received'