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_1564174
_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_absolute_configuration unk
_chemical_formula_moiety
'C52 H41.5 Br2 Cl N4 Na1.2 Ni O10, Cl O4, 0.5(C4 H10 O), 0.4(Na2)'
_chemical_formula_sum            'C54 H46.5 Br2 Cl2 N4 Na2 Ni O14.5'
_chemical_formula_weight         1318.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 104.6742(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1089(2)
_cell_length_b                   18.0820(3)
_cell_length_c                   16.6095(3)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.566
_cell_measurement_theta_min      2.368
_cell_volume                     2937.01(9)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0286
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39517
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         2.146
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.863
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6056
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       block
_exptl_crystal_F_000             1337
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
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 Flack x determined using 4089 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
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_refine_ls_abs_structure_Flack   0.028(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         10392
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0557P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    0.941
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                9504
_reflns_number_total             10392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            complex1R0.cif
_cod_data_source_block           uf15-1
_cod_original_formula_sum        'C54 H46.50 Br2 Cl2 N4 Na2 Ni O14.50'
_cod_database_code               1564174
_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
 C104-C103
 1.4 with sigma of 0.02
 C102-C101
 1.4 with sigma of 0.02
 C103-O15
 1.35 with sigma of 0.02
 C102-O15
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C104) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(C102)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq, Uanis(O12A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.02
Uanis(C101) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: H35(0.5) O13A(0.4) O14(0.6) O12(0.6) O15(0.5) C103(0.5) H10A(0.5)
 H10B(0.5) Na1(0.6) Na2A(0.6) C101(0.5) H10C(0.5) H10D(0.5) H10E(0.5) C102(0.5)
 H10F(0.5) H10G(0.5) Na1A(0.4) Na2(0.4) C104(0.5) H10H(0.5) H10I(0.5) H10J(0.5)
 O14A(0.4) O13(0.6) O12A(0.4)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C9(H9), C19(H19), C18(H18), C36(H36), C35(H35), C43(H43), C44(H44)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C39(H39A,H39B), C45(H45A,H45B), C103(H10A,
 H10B), C102(H10F,H10G)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C7(H7), C8(H8), C16(H16), C17(H17), C14(H14), C15(H15),
 C25(H25), C26(H26), C23(H23), C24(H24), C28(H28), C27(H27), C34(H34), C30(H30),
  C41(H41), C42(H42), C40(H40), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52)
5.d Idealised Me refined as rotating group:
 C101(H10C,H10D,H10E), C104(H10H,H10I,H10J)
5.e Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6A)
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_shelx_res_checksum              43429
_shelx_hkl_checksum              95405