Stability <i>vs.</i> activity in electrocatalytic hydrogen production and magnetic studies of mononuclear labile Cu(II) and Ni(II) complexes.
Bhatti, Maria A.; Carrella, Luca M.; Streb, Carsten; Rentschler, Eva; Sundaresan, Sriram; Dalton transactions (Cambridge, England : 2003) 55 (2026) 3866–3874; doi:10.1039/d6dt00175k

data_7720096
_publ_section_title
;
 Stability <i>vs.</i> activity in electrocatalytic hydrogen production and
 magnetic studies of mononuclear labile Cu(II) and Ni(II) complexes.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3866
_journal_page_last               3874
_journal_paper_doi               10.1039/d6dt00175k
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C96 H129.75 Co5 N9 O16, 0.25(C4 H9)'
_chemical_formula_sum            'C44 H52 Cu2 N4 O8'
_chemical_formula_weight         891.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-08-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-12-11 deposited with the CCDC.	2026-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7781(8)
_cell_length_b                   17.5851(8)
_cell_length_c                   6.8233(3)
_cell_measurement_reflns_used    61996
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.20
_cell_measurement_theta_min      2.32
_cell_volume                     2013.18(16)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.1, Darmstadt 2022
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_details
;
 1783 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  180
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            17977
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.465
_diffrn_reflns_theta_min         2.316
_diffrn_source                   'Axo Mo'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_target            Cu
_diffrn_source_type              'I\mS Incoatec'
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    1.116
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.6966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_exptl_crystal_size_rad          0.100
_refine_diff_density_max         2.158
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         3150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0843P)^2^+3.3531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1674
_reflns_d_resolution_high        0.662
_reflns_d_resolution_low         8.793
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              21
_reflns_limit_h_min              -24
_reflns_limit_k_max              26
_reflns_limit_k_min              -22
_reflns_limit_l_max              7
_reflns_limit_l_min              -9
_reflns_number_gt                2413
_reflns_number_total             3150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00175k2.cif
_cod_data_source_block           mb-001-03
_cod_depositor_comments
'Adding full bibliography for 7720096--7720097.cif.'
_cod_database_code               7720096
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C8(H8)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              43500
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   12.0
_stoe_evaluation_integration_b   0.9
_stoe_evaluation_integration_ems 0.032
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 86.2
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 4
_stoe_evaluation_lana_max_2theta_available 65.0
_stoe_evaluation_lana_max_2theta_desired 65.0
_stoe_evaluation_lana_mean_redundancy 5.7
_stoe_evaluation_lana_number_refls_after_or 17977
_stoe_evaluation_lana_number_refls_outliers 6060
_stoe_evaluation_lana_number_refls_total 24037
_stoe_evaluation_lana_number_refls_unique 3150
_stoe_evaluation_lana_number_refls_written 17977
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group mmm
_stoe_evaluation_lana_table
;
2Theta           7.6   14.4   21.2   28.0   34.8   41.6   48.4   55.2   62.0
<Resolution>    4.70   2.77   1.93   1.46   1.18   1.00   0.87   0.77   0.70
N(total)         327   1431   2717   3059   4360   4623   3769   3135    616
<Redundancy>    12.6   15.8   14.1    9.2    8.6    6.9    4.4    3.3    1.4
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0  100.0   98.0   45.5
<I/sigma>      297.8  158.7   76.5   61.7   32.9   19.8   11.7    6.5    3.8
R(int)         0.057  0.046  0.064  0.067  0.059  0.066  0.057  0.083  0.112
;
_stoe_measurement_identifier     MB-001-03
_stoe_measurement_max_exposure_per_frame '60.0 s'
_stoe_measurement_mean_exposure_per_frame '60.0 s'
_stoe_measurement_min_exposure_per_frame '60.0 s'
_stoe_measurement_total_exposure_time '29.7 h'
_stoe_measurement_total_frame_number 1783
_stoe_measurement_total_run_number 4
_stoe_measurement_tube_power     '49.8 W'