The structure and magnetism of mono- and di-nuclear Ni(ii) complexes derived from {N3O}-donor Schiff base ligands
Panja, Anangamohan; Jana, Narayan Ch.; Adak, Sarmistha; Brandão, Paula; Dlháň, Lubor; Titiš, Ján; Boča, Roman; New J. Chem. 41 (2017) 3143–; doi:10.1039/C7NJ00158D

data_7056073
_publ_section_title
;
 The structure and magnetism of mono- and di-nuclear Ni(ii) complexes
 derived from {N3O}-donor Schiff base ligands
;
_journal_issue                   8
_journal_name_full               'New J. Chem.'
_journal_page_first              3143
_journal_paper_doi               10.1039/C7NJ00158D
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C30 H48 N6 Ni O2, 2(Cl O4)'
_chemical_formula_sum            'C30 H48 Cl2 N6 Ni O10'
_chemical_formula_weight         782.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-03-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-14 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.814(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9692(4)
_cell_length_b                   9.8140(4)
_cell_length_c                   20.2915(7)
_cell_measurement_reflns_used    410
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      3.15
_cell_volume                     1748.30(12)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick,2013)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35922
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.409
_diffrn_reflns_theta_min         2.051
_exptl_absorpt_coefficient_mu    0.771
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       Block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0020(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3589
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+1.7375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2817
_reflns_number_total             3589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00158d2.cif
_cod_data_source_block           complex-1
_cod_depositor_comments
'Adding full bibliography for 7056073--7056077.cif.'
_cod_database_code               7056073
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.802
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2-O3 \\sim Cl2-O4 \\sim Cl2-O5 \\sim Cl2-O6
 with sigma of 0.02
 O3-O5 \\sim O4-O6 \\sim O3-O6 \\sim O4-O5 \\sim O3-O4 \\sim O5-O6
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim O3 \\sim O4 \\sim O5 \\sim O6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 Cl2, O3, O4, O5, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C0AA, C1AA, C2AA, N4AA, C3AA, C14, C1AA, C0AA, C2AA, C1AA, N4AA, C2AA, N4AA,
 C3AA, N4AA, C14, N13A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N13B, C5AA, C7AA, C8AA, C0BA, N9AA, C6AA, N13B, C6AA, C7AA, C6AA, C8AA, C7AA,
 N9AA, C8AA, N9AA, C5AA, N9AA, C0BA, C5AA, C5AA, C5AA, C7AA, C7AA, C8AA, C0BA,
 C0BA, C0BA, C6AA, C6AA, N13B, C5AA, C8AA, C0BA, N9AA, C0BA, C5AA, N9AA, C0BA,
 N9AA, N13B, N13B, C8AA, N13B, N13B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: H12C(0.45) H12D(0.45) H12A(0.55) H12B(0.55) N13B(0.45) C0AA(0.55)
 H0AA(0.55) H0AB(0.55) C1AA(0.55) H1AA(0.55) H1AB(0.55) C2AA(0.55) H2AA(0.55)
 H2AB(0.55) N4AA(0.55) H4AA(0.55) C5AA(0.45) H5AA(0.45) H5AB(0.45) H5AC(0.45)
 C3AA(0.55) H3AA(0.55) H3AB(0.55) H3AC(0.55) C7AA(0.45) H7AA(0.45) H7AB(0.45)
 C8AA(0.45) H8AA(0.45) H8AB(0.45) C0BA(0.45) H0BA(0.45) H0BB(0.45) H0BC(0.45)
 N9AA(0.45) H9AA(0.45) C6AA(0.45) H6AA(0.45) H6AB(0.45) N13A(0.55) C14(0.55)
 H14A(0.55) H14B(0.55) H14C(0.55) Ni1A(0.45) Ni1(0.05)
6.a Ternary CH refined with riding coordinates:
 N4AA(H4AA), N9AA(H9AA)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12C,H12D), C12(H12A,H12B), C0AA(H0AA,
 H0AB), C1AA(H1AA,H1AB), C2AA(H2AA,H2AB), C7AA(H7AA,H7AB), C8AA(H8AA,H8AB),
 C6AA(H6AA,H6AB)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8)
6.d Idealised Me refined as rotating group:
 C5AA(H5AA,H5AB,H5AC), C3AA(H3AA,H3AB,H3AC), C0BA(H0BA,H0BB,H0BC), C14(H14A,
 H14B,H14C)
;
_shelx_res_checksum              31494
_olex2_submission_special_instructions 'No special instructions were received'