A tetranuclear nickel cluster isolated in multiple high-valent states.
Jacob, Samuel I.; Douair, Iskander; Wu, Guang; Maron, Laurent; Ménard, Gabriel; Chemical communications (Cambridge, England) 56 (2020) 8182–8185; doi:10.1039/d0cc01699c

data_7126376
_publ_section_title
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 A tetranuclear nickel cluster isolated in multiple high-valent states.
;
_journal_issue                   59
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8182
_journal_page_last               8185
_journal_paper_doi               10.1039/d0cc01699c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C82 H60 N8 Ni4 O6'
_chemical_formula_sum            'C82 H60 N8 Ni4 O6'
_chemical_formula_weight         1488.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2020-01-15 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                107.838(9)
_cell_angle_beta                 105.170(9)
_cell_angle_gamma                95.623(9)
_cell_formula_units_Z            2
_cell_length_a                   13.084(6)
_cell_length_b                   15.980(8)
_cell_length_c                   22.737(11)
_cell_measurement_reflns_used    1285
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.55
_cell_measurement_theta_min      2.33
_cell_volume                     4285(4)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      99.96
_diffrn_measured_fraction_theta_full 0.9603
_diffrn_measured_fraction_theta_max 0.9603
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1066
_diffrn_reflns_av_unetI/netI     0.2592
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21757
_diffrn_reflns_theta_full        24.7130
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         0.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.915
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0743 before and 0.0484 after correction.
The Ratio of minimum to maximum transmission is 0.7038.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.1534
_exptl_crystal_description       needle
_exptl_crystal_F_000             1539.3632
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.2422
_refine_diff_density_min         -1.6401
_refine_diff_density_rms         0.2619
_refine_ls_d_res_high            0.8500
_refine_ls_d_res_low             20.5926
_refine_ls_goodness_of_fit_ref   0.9182
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    109
_refine_ls_number_parameters     887
_refine_ls_number_reflns         14042
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.9175
_refine_ls_R_factor_all          0.1716
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.0066
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0838P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.2089
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -18
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                5998
_reflns_number_total             14042
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0cc01699c2.cif
_cod_data_source_block           149_Ni_2_0m_a
_cod_depositor_comments
;
Adding full bibliography for 7126375--7126378.cif.

2025-03-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '0.5(C82 H60 N8 Ni4 O6)'
_cod_original_formula_sum        'C41 H30 N4 Ni2 O3'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     744.11
_cod_database_code               7126376
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N00H-H00H
 1 with sigma of 0.01
 N00H-H00H \\sim N00D-H00D \\sim N00G-H00G \\sim N2-H2
 with sigma of 0.01
 H00H-Ni4 \\sim H00H-Ni2 \\sim H00D-Ni3 \\sim H00D-Ni01 \\sim H00G-Ni01 \\sim
H00G-Ni4
 with sigma of 0.01
 H00H-Ni4 \\sim H2-Ni2 \\sim H2-Ni3
 with sigma of 0.01
 H00H-C017 \\sim H00D-C00V \\sim H00G-C015 \\sim H2-C01P
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C00P) = Uanis(C00T)
Uanis(N00E) = Uanis(N00I)
Uanis(C01A) = Uanis(C01G)
Uanis(C00K) = Uanis(C016)
Uanis(C010) = Uanis(C01X)
4. Others
 Fixed Uiso: H00H(0.1) H00D(0.1) H00G(0.1) H2(0.1)
5.a Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00N(H00N), C00P(H00P), C00S(H00S), C00T(H00T), C00W(H00W),
 C010(H010), C014(H014), C019(H019), C01B(H01B), C01C(H01C), C01H(H01H),
 C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N),
 C01R(H01R), C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V), C01W(H01W),
 C01X(H01X), C01Y(H01Y), C01Z(H01Z), C022(H022), C024(H024), C025(H025),
 C02B(H02B), C02C(H02C), C02D(H02D), C02E(H02E), C02G(H02G), C02H(H02H),
 C02I(H02I), C02K(H02K), C02L(H02L), C02M(H02M), C02N(H02N), C02R(H02R),
 C02S(H02S), C02V(H02w)
5.b Idealised Me refined as rotating group:
 C02P(H02a,H02f,H02j), C02T(H02o,H02p,H02q), C02U(H02t,H02u,H02v), C02X(H02x,
 H02y,H)
;
_olex2_submission_special_instructions 'No special instructions were received'