Tetranuclear Ni<sup>II</sup>-Mannich base complex with oxygenase, water splitting and ferromagnetic and antiferromagnetic coupling properties.
Patra, Arka; Das, Avijit; Sarkar, Abhimanyu; Gómez-García, Carlos J; Sinha, Chittaranjan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13515–13528; doi:10.1039/d4dt01425a

data_7716780
_publ_section_title
;
 Tetranuclear Ni<sup>II</sup>-Mannich base complex with oxygenase, water
 splitting and ferromagnetic and antiferromagnetic coupling properties.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13515
_journal_page_last               13528
_journal_paper_doi               10.1039/d4dt01425a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C44 H64 Cl1.7 N4 Ni4 O12, 2(Cl)'
_chemical_formula_sum            'C44 H64 Cl3.7 N4 Ni4 O12'
_chemical_formula_weight         1206.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-03-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-05-12 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.786(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3672(11)
_cell_length_b                   13.5893(11)
_cell_length_c                   15.9512(13)
_cell_measurement_reflns_used    9308
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.20
_cell_volume                     2743.2(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0569
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            73292
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.199
_exptl_absorpt_coefficient_mu    1.590
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   0.909
_exptl_transmission_factor_min   0.875
_refine_diff_density_max         0.835
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         9600
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+6.1685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                8464
_reflns_number_total             9600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01425a2.cif
_cod_data_source_block           pkm_arka1_0m_b_pl
_cod_depositor_comments
'Adding full bibliography for 7716779--7716780.cif.'
_cod_original_formula_sum        'C44 H64 Cl3.70 N4 Ni4 O12'
_cod_database_code               7716780
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.56(2)
 0.44(2)
2. 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
3. Restrained distances
 O11-H11A = O11-H11B
 0.85 with sigma of 0.02
 O12-H12A = O12-H12B
 0.85 with sigma of 0.02
 H11A-H11B
 1.34 with sigma of 0.04
 H12A-H12B
 1.34 with sigma of 0.04
 Ni2-H11A \\sim Ni2-H11B
 with sigma of 0.02
 Ni2-H12A \\sim Ni2-H12B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq: with sigma of 0.0001 and sigma for
terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 Cl1, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Cl1(0.9) Cl2(0.8)
7.a Riding coordinates:
 O9(H9A,H9B), O10(H10A,H10B)
7.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10C,H10D), C11(H11C,H11D), C12(H12C,H12D), C13(H13A,H13B),
 C14(H14A,H14B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
  C35(H35A,H35B), C36(H36A,H36B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C16(H16), C18(H18), C25(H25), C27(H27), C38(H38), C40(H40)
7.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9C,H9D,H9E), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C)
;
_shelx_res_checksum              11244
_shelx_fab_checksum              52202
_olex2_submission_special_instructions 'No special instructions were received'