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_1564175
_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_moiety         'C58 H52 Br2 N4 Na0.33 Ni4 O12, 1.67(Na1)'
_chemical_formula_sum            'C58 H52 Br2 N4 Na2 Ni4 O12'
_chemical_formula_weight         1437.67
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   44.4417(10)
_cell_length_b                   44.4417(10)
_cell_length_c                   11.3230(3)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    100
_cell_measurement_theta_max      17.29
_cell_measurement_theta_min      2.28
_cell_volume                     19367.5(8)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.383
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.383
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            48229
_diffrn_reflns_point_group_measured_fraction_full 0.382
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         18.070
_diffrn_reflns_theta_min         1.833
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.844
_exptl_absorpt_correction_T_max  0.7442
_exptl_absorpt_correction_T_min  0.5683
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             6552
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Flack x determined using 2639 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         5947
_refine_ls_number_restraints     315
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0967P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.382
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5653
_reflns_number_total             5947
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            complex2R0.cif
_cod_data_source_block           kyj156-5
_cod_original_cell_volume        19367.5(10)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               1564175
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.458(3)
 0.542(3)
2. 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
3. Restrained distances
 C6-C17
 1.35 with sigma of 0.02
 Na59-Na13
 1.4 with sigma of 0.02
4. Rigid bond restraints
 C45, C46, C47, C48, C49, C50
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C11, C12, C13, C0AA, C15, C16
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
C11 \\sim C12 \\sim C13 \\sim C0AA \\sim C15 \\sim C16: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C36) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq,
Uanis(C31) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(C54) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(Na60)
\\sim Ueq, Uanis(Na14) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Na59) \\sim Ueq, Uanis(Na13) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Na1) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Others
 Fixed Sof: Na13(0.33333) Na59(0.33333) Na14(0.33333) Na60(0.33333) Na1(0.33333)
7.a Ternary CH refined with riding coordinates:
 C8(H8), C9(H9), C18(H18), C26(H26), C34(H34), C42(H42), C44(H44), C52(H52)
7.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C25(H25A,H25B), C41(H41A,H41B), C51(H51A,H51B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C12(H12), C13(H13), C0AA(H0AA), C15(H15), C17(H17),
 C20(H20), C21(H21), C22(H22), C23(H23), C29(H29), C31(H31), C33(H33), C36(H36),
  C37(H37), C38(H38), C39(H39), C43(H43), C46(H46), C47(H47), C48(H48), C49(H49)
7.d Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C11(C12,C13,C0AA,C15,C16), C19(C20,C21,C22,C23,C24),
 C35(C36,C37,C38,C39,C40)
7.e Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C)
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_shelx_res_checksum              83534
_shelx_hkl_checksum              57581