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_7126377
_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
'0.5(C82 H60 N8 Ni4 O6), 1.5(C Cl2), 5(C), B C24 F20'
_chemical_formula_sum            'C71.5 H30 B Cl3 F20 N4 Ni2 O3'
_chemical_formula_weight         1607.60
_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
_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                87.662(12)
_cell_angle_beta                 78.355(15)
_cell_angle_gamma                89.016(17)
_cell_formula_units_Z            4
_cell_length_a                   17.673(9)
_cell_length_b                   19.000(9)
_cell_length_c                   19.530(8)
_cell_measurement_reflns_used    1274
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.07
_cell_measurement_theta_min      2.38
_cell_volume                     6417(5)
_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)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.9455
_diffrn_measured_fraction_theta_max 0.9455
_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  0.0443
_diffrn_reflns_av_unetI/netI     0.1041
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38440
_diffrn_reflns_theta_full        26.8534
_diffrn_reflns_theta_max         26.85
_diffrn_reflns_theta_min         1.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'brownish yellow'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.6637
_exptl_crystal_description       plate
_exptl_crystal_F_000             3218.8535
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         5.1714
_refine_diff_density_min         -3.2013
_refine_diff_density_rms         0.2959
_refine_ls_d_res_high            0.7867
_refine_ls_d_res_low             19.1142
_refine_ls_goodness_of_fit_ref   1.0956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    107
_refine_ls_number_parameters     1823
_refine_ls_number_reflns         26110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0956
_refine_ls_R_factor_all          0.1639
_refine_ls_R_factor_gt           0.1084
_refine_ls_shift/su_max          0.0173
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1869P)^2^+49.8567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3016
_refine_ls_wR_factor_ref         0.3499
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -21
_reflns_limit_k_max              24
_reflns_limit_k_min              -23
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                16261
_reflns_number_total             26110
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0cc01699c2.cif
_cod_data_source_block           339_DioxidizedNi4_0m
_cod_depositor_comments
'Adding full bibliography for 7126375--7126378.cif.'
_cod_original_cell_volume        6418(5)
_cod_database_code               7126377
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All H(H,H) groups, All C(H,H,H) groups
2. Others
 Fixed Sof: C145(0.5) C143(0.5) C11(0.5) C12(0.5) C13(0.5) C14(0.5)
 Fixed Uiso: H0aa(0.05) H03A(0.05) H04J(0.05) H05a(0.05) H20a(0.05)
3.a Ternary CH refined with riding coordinates:
 N3(H3), N4(H4), N1(H1), N7(H7a)
3.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C15(H15), C8(H8), C2aa(H2aa), C18(H18), C7(H7), C19(H19),
 C02F(H02F), C02I(H02I), C02K(H02K), C02P(H02P), C02S(H02S), C02T(H02T),
 C02U(H02U), C02X(H02X), C02Z(H02Z), C035(H035), C037(H037), C038(H038),
 C03A(H03A), C03H(H03H), C03P(H03P), C03R(H03R), C03T(H03T), C03U(H03U),
 C03Y(H03Y), C041(H041), C044(H044), C048(H048), C04C(H04C), C04E(H04E),
 C04H(H04H), C04I(H04I), C04J(H04J), C04K(H04K), C04L(H04L), C04M(H04M),
 C04P(H04P), C04V(H04V), C04Y(H04Y), C058(H058), C059(H059), C05F(H05F),
 C05I(H05I)
3.c Idealised Me refined as rotating group:
 C0aa(H0aa,H0ab,H0ac), C04W(H04a,H04b,H04d), C05K(H05a,H05b,H05c), C20(H20a,
 H20b,H20c)
;
_olex2_submission_special_instructions 'No special instructions were received'