Improvement of electrocatalytic water oxidation activity of novel copper complex by modulating the axial coordination of phosphate on metal center.
Wang, Jieying; Ping, Yezi; Chen, Yanmei; Liu, Shanshan; Dong, Jinfeng; Ruan, Zhijun; Liang, Xiangming; Lin, Junqi; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5222–5229; doi:10.1039/d3dt03409g

data_7715165
_publ_section_title
;
 Improvement of electrocatalytic water oxidation activity of novel copper
 complex by modulating the axial coordination of phosphate on metal
 center.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5222
_journal_page_last               5229
_journal_paper_doi               10.1039/d3dt03409g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C16 H22 Cl Cu N4 O4, Cl O4'
_chemical_formula_sum            'C16 H22 Cl2 Cu N4 O8'
_chemical_formula_weight         532.81
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-26
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-01-29 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3806(4)
_cell_length_b                   11.9359(4)
_cell_length_c                   12.9332(5)
_cell_measurement_reflns_used    9634
_cell_measurement_temperature    192.00
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.32
_cell_volume                     2065.55(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      192.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0793
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43215
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.388
_diffrn_reflns_theta_min         2.190
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2218
_refine_ls_number_restraints     289
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0329P)^2^+1.7822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1956
_reflns_number_total             2218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03409g2.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7715165--7715166.cif.
;
_cod_database_code               7715165
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.762
_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
2. Restrained distances
 Cl1-O1 \\sim Cl1-O4 \\sim Cl1-O2 \\sim Cl1-O3
 with sigma of 0.02
 O1-O2 \\sim O1-O3 \\sim O1-O4 \\sim O2-O3 \\sim O2-O4 \\sim O3-O4
 with sigma of 0.02
 O5-O6 \\sim O5-O7 \\sim O5-O8 \\sim O6-O7 \\sim O6-O8 \\sim O7-O8
 with sigma of 0.02
 Cl2-O8 \\sim Cl2-O6 \\sim Cl2-O5 \\sim Cl2-O7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim Cl1A \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O7
\\sim O6 \\sim O1A \\sim O2A \\sim O3A \\sim O4A \\sim O8: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Same fragment restrains
{Cl1A, O1A, O2A, O3A, O4A} sigma for 1-2: 0.02, 1-3: 0.02
as in
{Cl1, O1, O2, O3, O4}
5. Others
 Sof(Cl1A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=0.5*(1-FVAR(2))
 Sof(Cl1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=0.5*FVAR(2)
 Fixed Sof: O7(0.5) O6(0.5) O8(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6)
6.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              40407
_olex2_submission_special_instructions 'No special instructions were received'