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_7126375
_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 H59 N8 Ni4 O6, 4(C H2 Cl2), C3 H3, F6 P'
_chemical_formula_sum            'C89 H70 Cl8 F6 N8 Ni4 O6 P'
_chemical_formula_weight         2010.96
_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             2019-12-15
_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                112.704(2)
_cell_angle_beta                 92.701(3)
_cell_angle_gamma                103.281(3)
_cell_formula_units_Z            2
_cell_length_a                   14.2332(15)
_cell_length_b                   16.4798(17)
_cell_length_c                   19.285(2)
_cell_measurement_reflns_used    1591
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      17.8
_cell_measurement_theta_min      2.54
_cell_volume                     4014.6(7)
_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      109.99
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.1472
_diffrn_reflns_av_unetI/netI     0.2996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28568
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        24.8260
_diffrn_reflns_theta_max         24.826
_diffrn_reflns_theta_min         1.158
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0756 before and 0.0610 after correction.
The Ratio of minimum to maximum transmission is 0.7928.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.6634
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056.2096
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.3704
_refine_diff_density_min         -2.4123
_refine_diff_density_rms         0.4736
_refine_ls_d_res_high            0.8464
_refine_ls_d_res_low             17.5856
_refine_ls_goodness_of_fit_ref   1.0202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    133
_refine_ls_number_parameters     1073
_refine_ls_number_reflns         13601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0202
_refine_ls_R_factor_all          0.2391
_refine_ls_R_factor_gt           0.0905
_refine_ls_shift/su_max          0.0171
_refine_ls_shift/su_mean         0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0699P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.2162
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              -19
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                5496
_reflns_number_total             13601
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0cc01699c2.cif
_cod_data_source_block           final
_cod_depositor_comments
'Adding full bibliography for 7126375--7126378.cif.'
_cod_database_code               7126375
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C50) = Uanis(C53)
Uanis(C1) = Uanis(C32)
Uanis(C5) = Uanis(C8)
Uanis(N6) = Uanis(N1)
Uanis(C69) = Uanis(C58)
3.a Ternary CH refined with riding coordinates:
 N6(H6a), N1(H1), N4(H4), N5(H5a)
3.b Secondary CH2 refined with riding coordinates:
 C83(H83a,H83b), C84(H84a,H84b), C85(H85a,H85b), C86(H86a,H86b)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31),
  C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C45(H45),
 C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C58(H58), C59(H59),
  C60(H60), C67(H67), C68(H68), C69(H69), C71(H71), C72(H72), C75(H75),
 C76(H76), C78(H78), C79(H79), C80(H80), C81(H81), C87(H87), C88(H88), C89(H89)
3.d Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C22(H22a,H22b,H22c), C62(H62a,H62b,H62c), C63(H63a,H63b,
 H63c)
;
_olex2_submission_special_instructions 'No special instructions were received'