Multinuclear nickel(II) complexes with chiral schiff base ligand
Farwa, Ume; Pait, Moumita; Ryu, Ji Yeon; Byun, Yong Min; Lee, Seul Gi; Jeong, Seung Hoo; Singh, Ovender; Singh, Neetu; Park, Hyoung-Ryun; Lee, Junseong; Inorganica Chimica Acta 511 (2020) 119798–; doi:10.1016/j.ica.2020.119798

data_1564176
_publ_section_title
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 Multinuclear nickel(II) complexes with chiral schiff base ligand
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_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119798
_journal_paper_doi               10.1016/j.ica.2020.119798
_journal_volume                  511
_journal_year                    2020
_chemical_formula_sum            'C105.48 H139.19 Cl2.5 N6 Na1.5 Ni6 O37.75'
_chemical_formula_weight         2570.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7935(4)
_cell_length_b                   20.7861(6)
_cell_length_c                   41.1035(12)
_cell_measurement_reflns_used    9237
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.922
_cell_measurement_theta_min      2.593
_cell_volume                     12639.3(6)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_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  0.0713
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            88788
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.387
_diffrn_reflns_theta_min         1.761
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.011
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5384
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       block
_exptl_crystal_F_000             5372
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
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 Flack x determined using 6166 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
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_refine_ls_abs_structure_Flack   0.026(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1666
_refine_ls_number_reflns         22862
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          2.234
_refine_ls_shift/su_mean         0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1557
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                16966
_reflns_number_total             22862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            complex3.cif
_cod_data_source_block           pait09-1
_cod_original_formula_sum        'C105.48 H139.19 Cl2.50 N6 Na1.50 Ni6 O37.75'
_cod_database_code               1564176
_olex2_refinement_description
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1. 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) groups
2. Restrained distances
 O31-O32
 2.2 with sigma of 0.02
 C111-O45
 1.35 with sigma of 0.02
 O46-C113
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9A) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C10A)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C8A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C69) \\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O32) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C107) \\sim Ueq, Uanis(C70) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C105) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C103) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O31) \\sim Ueq, Uanis(O32) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C68) \\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O40) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O45) \\sim Ueq, Uanis(C111) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C113) \\sim Ueq, Uanis(Na2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C111) \\sim Ueq, Uanis(O46) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: O40(0.75) H40(0.75) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C9(0.5)
 H9A(0.5) H9B(0.5) H9C(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5) C9A(0.5)
 H9AA(0.5) H9AB(0.5) H9AC(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
 C68(0.33333) H68A(0.33333) H68B(0.33333) H68C(0.33333) C69(0.33333)
 H69A(0.33333) H69B(0.33333) H69C(0.33333) C70(0.33333) H70A(0.33333)
 H70B(0.33333) H70C(0.33333) C68A(0.66) H68D(0.66) H68E(0.66) H68F(0.66)
 C69A(0.66) H69D(0.66) H69E(0.66) H69F(0.66) C70A(0.66) H70D(0.66) H70E(0.66)
 H70F(0.66) O34(0.75) H34(0.75) O33(0.75) H33A(0.75) C101(0.75) H10J(0.75)
 H10K(0.75) H10L(0.75) O35(0.5) H35A(0.5) O36(0.5) H36(0.5) O39(0.5) H39(0.5)
 C104(0.5) H10P(0.5) H10Q(0.5) H10R(0.5) C107(0.25) H10S(0.25) H10T(0.25)
 H10U(0.25) O41(0.5) H41A(0.5) C109(0.5) H10V(0.5) H10W(0.5) H10X(0.5) O37(0.5)
 H37(0.5) C105(0.5) H10Y(0.5) H(0.5) HA(0.5) C103(0.5) H10M(0.5) H10N(0.5)
 H10O(0.5) C10A(0.5) H10D(0.5) H10E(0.5) H10F(0.5) C112(0.75) H11D(0.75)
 H11E(0.75) H11F(0.75) C108(0.75) H10G(0.75) H10H(0.75) H10I(0.75) Na1(0.75)
 Cl1(0.5) O30(0.5) O29(0.5) O32(0.5) O31(0.5) O45(0.75) H45(0.75) C111(0.75)
 H11G(0.75) H11H(0.75) H11I(0.75) O46(0.25) H46(0.25) C113(0.25) H11J(0.25)
 H11K(0.25) H11L(0.25) Na4(0.5) Na2(0.125) Na3(0.125)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C13(H13), C22(H22), C23(H23), C42(H42), C43(H43), C52(H52),
 C53(H53), C72(H72), C73(H73), C82(H82), C83(H83)
5.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C24(H24A,H24B), C44(H44A,H44B), C54(H54A,H54B), C74(H74A,
 H74B), C84(H84A,H84B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C11(H11), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
 C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C35(H35), C41(H41), C47(H47),
  C48(H48), C49(H49), C50(H50), C51(H51), C57(H57), C58(H58), C59(H59),
 C63(H63), C65(H65), C71(H71), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81),
  C87(H87), C88(H88), C89(H89), C90(H90)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC),
 C10(H10A,H10B,H10C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C),
 C68A(H68D,H68E,H68F), C69A(H69D,H69E,H69F), C70A(H70D,H70E,H70F), C92(H92A,
 H92B,H92C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C),
 C96(H96A,H96B,H96C), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C), C110(H11A,H11B,
 H11C), C1AA(H1AA,H1AB,H1AC), C101(H10J,H10K,H10L), C104(H10P,H10Q,H10R),
 C107(H10S,H10T,H10U), C109(H10V,H10W,H10X), C105(H10Y,H,HA), C103(H10M,H10N,
 H10O), C10A(H10D,H10E,H10F), C112(H11D,H11E,H11F), C108(H10G,H10H,H10I),
 C111(H11G,H11H,H11I), C113(H11J,H11K,H11L)
5.e Idealised tetrahedral OH refined as rotating group:
 O40(H40), O43(H43A), O42(H42A), O34(H34), O33(H33A), O35(H35A), O36(H36),
 O39(H39), O41(H41A), O37(H37), O45(H45), O46(H46)
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