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_7126378
_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, 6(C H2 Cl2), 4(B C24 F20)'
_chemical_formula_sum            'C184 H72 B4 Cl12 F80 N8 Ni4 O6'
_chemical_formula_weight         4714.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_Int_Tables_number      13
_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                90
_cell_angle_beta                 90.382(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.9020(12)
_cell_length_b                   28.1020(16)
_cell_length_c                   19.0679(11)
_cell_measurement_reflns_used    5846
_cell_measurement_temperature    99.96
_cell_measurement_theta_max      23.30
_cell_measurement_theta_min      2.28
_cell_volume                     9592.5(10)
_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      99.96
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9947
_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  0.1285
_diffrn_reflns_av_unetI/netI     0.1526
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54230
_diffrn_reflns_theta_full        24.7813
_diffrn_reflns_theta_max         24.78
_diffrn_reflns_theta_min         0.72
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4980
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.6319
_exptl_crystal_description       plate
_exptl_crystal_F_000             4682.2420
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.7736
_refine_diff_density_min         -2.2013
_refine_diff_density_rms         0.2902
_refine_ls_d_res_high            0.8478
_refine_ls_d_res_low             28.1020
_refine_ls_goodness_of_fit_ref   1.2705
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    66
_refine_ls_number_parameters     1295
_refine_ls_number_reflns         16400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.2705
_refine_ls_R_factor_all          0.2041
_refine_ls_R_factor_gt           0.1122
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3049
_refine_ls_wR_factor_ref         0.4050
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -21
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              -14
_reflns_number_gt                8030
_reflns_number_total             16400
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0cc01699c2.cif
_cod_data_source_block           335_Try6_0m_a
_cod_depositor_comments
'Adding full bibliography for 7126375--7126378.cif.'
_cod_original_sg_symbol_Hall     '-P 2yc (x-z,y,z)'
_cod_database_code               7126378
_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(C028) = Uanis(C022)
3.a Ternary CH refined with riding coordinates:
 N3(H3), N4(H4)
3.b Secondary CH2 refined with riding coordinates:
 C04B(H04d,H04e), C101(H10a,H10b), C100(H10c,H10d)
3.c Aromatic/amide H refined with riding coordinates:
 C01Q(H01Q), C01T(H01T), C01Y(H01Y), C020(H020), C022(H022), C024(H024),
 C025(H025), C028(H028), C029(H029), C02H(H02H), C02R(H02R), C02S(H02S),
 C02Y(H02Y), C031(H031), C032(H032), C034(H034), C035(H035), C037(H037),
 C038(H038), C03G(H03G), C03J(H03J), C041(H041)
3.d Idealised Me refined as rotating group:
 C03X(H03a,H03b,H03c), C042(H04a,H04b,H04c)
;
_olex2_submission_special_instructions 'No special instructions were received'