Impact of the hybridization form of the coordinated nitrogen atom on the electrocatalytic water oxidation performance of copper complexes with pentadentate amine-pyridine ligands.
Yu, Kaishan; Wang, Tao; Sun, Yue; Kang, Mei; Wang, Xinxin; Zhu, Dingwei; Xue, Siyi; Shen, Junyu; Zhang, Qijian; Liu, Jinxuan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 612–618; doi:10.1039/d3dt03185c

data_7714574
_publ_section_title
;
 Impact of the hybridization form of the coordinated nitrogen atom on the
 electrocatalytic water oxidation performance of copper complexes with
 pentadentate amine-pyridine ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              612
_journal_page_last               618
_journal_paper_doi               10.1039/d3dt03185c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C19 H29 Cu N5, 2(B F4)'
_chemical_formula_sum            'C19 H29 B2 Cu F8 N5'
_chemical_formula_weight         564.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-10-31
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-01 deposited with the CCDC.	2023-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.422(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.2265(18)
_cell_length_b                   25.288(3)
_cell_length_c                   14.4222(19)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.64
_cell_measurement_theta_min      2.21
_cell_volume                     4922.6(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1014
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            83272
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.708
_diffrn_reflns_theta_min         1.611
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0856 before and 0.0561 after correction.
The Ratio of minimum to maximum transmission is 0.8117.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         11442
_refine_ls_number_restraints     310
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.0856
_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^)+(0.0744P)^2^+9.1913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7451
_reflns_number_total             11442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03185c2.cif
_cod_data_source_block           ok_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7714573--7714574.cif.'
_cod_original_cell_volume        4922.7(11)
_cod_database_code               7714574
_shelx_shelxl_version_number     2018/3
_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
 F2-F17
 2.2 with sigma of 0.01
 F5-B2 \\sim F20-B2
 with sigma of 0.02
 F8-B2 \\sim F22-B2
 with sigma of 0.02
 B2-F6 \\sim B2-F19
 with sigma of 0.02
 B2-F7 \\sim B2-F21
 with sigma of 0.02
 F6-B2 \\sim F19-B2
 with sigma of 0.02
 F7-B2 \\sim F21-B2
 with sigma of 0.02
 F20-B2 \\sim F5-B2
 with sigma of 0.02
 F22-B2 \\sim F8-B2
 with sigma of 0.02
 F11-B3 \\sim F24-B3
 with sigma of 0.02
 F10-B3 \\sim F25-B3
 with sigma of 0.02
 B3-F9 \\sim B3-F1A
 with sigma of 0.02
 F25-B3 \\sim F10-B3
 with sigma of 0.02
 F24-B3 \\sim F11-B3
 with sigma of 0.02
 F12-B3 \\sim F23-B3
 with sigma of 0.02
 F9-B3 \\sim F1A-B3
 with sigma of 0.02
 F15-B4 \\sim F28-B4
 with sigma of 0.02
 F14-B4 \\sim F27-B4
 with sigma of 0.02
 F16-B4 \\sim F26-B4
 with sigma of 0.02
 F28-B4 \\sim F15-B4
 with sigma of 0.02
 F13-B4 \\sim F29-B4
 with sigma of 0.02
 F3-B1 \\sim F17-B1
 with sigma of 0.02
 F17-B1 \\sim F3-B1
 with sigma of 0.02
 F4-B1 \\sim F18-B1
 with sigma of 0.02
3. Rigid bond restraints
 F25, B3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
F7 \\sim F6 \\sim F8 \\sim B2 \\sim F5: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
F5 \\sim F7 \\sim F8 \\sim F6: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
F21 \\sim F22 \\sim F19 \\sim B2 \\sim F20: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
F11 \\sim F12 \\sim F9 \\sim F10: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
F25 \\sim F1A \\sim F23 \\sim F24: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
F14 \\sim B4 \\sim F13 \\sim F15 \\sim F16: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
F29 \\sim F27 \\sim F26 \\sim F28 \\sim B4: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
F3 \\sim F4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
F18 \\sim F17: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(F7) \\sim Ueq, Uanis(B2) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F8) \\sim
Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(F7) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F6) \\sim
Ueq, Uanis(B2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F5) \\sim
Ueq, Uanis(B2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(F21) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F20)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F25) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F1A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F13) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(B4) \\sim Ueq, Uanis(F14)
\\sim Ueq, Uanis(F16) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(F27) \\sim Ueq, Uanis(B4) \\sim Ueq, Uanis(F26) \\sim Ueq, Uanis(F29)
\\sim Ueq, Uanis(F28) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(F4) \\sim Ueq, Uanis(F3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F18) \\sim Ueq, Uanis(F17) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(F21)=Sof(F22)=Sof(F19)=Sof(F20)=1-FVAR(1)
 Sof(F5)=Sof(F8)=Sof(F6)=Sof(F7)=FVAR(1)
 Sof(F24)=Sof(F23)=Sof(F25)=Sof(F1A)=1-FVAR(2)
 Sof(F12)=Sof(F11)=Sof(F10)=Sof(F9)=FVAR(2)
 Sof(F28)=Sof(F26)=Sof(F29)=Sof(F27)=1-FVAR(3)
 Sof(F15)=Sof(F13)=Sof(F16)=Sof(F14)=FVAR(3)
 Sof(F17)=Sof(F18)=1-FVAR(4)
 Sof(F3)=Sof(F4)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C33(H33A,H33B), C25(H25A,H25B), C13(H13A,H13B),
 C31(H31A,H31B), C28(H28A,H28B), C8(H8A,H8B), C11(H11A,H11B), C30(H30A,H30B),
 C27(H27A,H27B), C10(H10A,H10B)
6.b Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C9(H9A,H9B,
 H9C), C29(H29A,H29B,H29C), C12(H12A,H12B,H12C)
6.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C38(H38), C23(H23), C37(H37), C20(H20), C21(H21), C2(H2), C4(H4),
 C3(H3), C22(H22), C1(H1), C17(H17), C15(H15), C35(H35), C36(H36), C16(H16)
;
_shelx_res_checksum              84114
_olex2_submission_special_instructions 'No special instructions were received'