Tetranuclear cobalt(II) and nickel(II) complexes with an unsymmetrical salamo-like ligand: Structural characterization, Hirshfeld analysis and fluorescent properties
Pu, Lu-Mei; Yu, Meng; Zhang, Yu; Long, Hai-Tao; Xu, Wei-Bing; Dong, Wen-Kui; Inorganica Chimica Acta 500 (2020) 119238–; doi:10.1016/j.ica.2019.119238

data_1565644
_publ_section_title
;
 Tetranuclear cobalt(II) and nickel(II) complexes with an unsymmetrical
 salamo-like ligand: Structural characterization, Hirshfeld analysis and
 fluorescent properties
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119238
_journal_paper_doi               10.1016/j.ica.2019.119238
_journal_volume                  500
_journal_year                    2020
_chemical_formula_moiety         'C44 H48 N6 Ni4 O18'
_chemical_formula_sum            'C44 H48 N6 Ni4 O18'
_chemical_formula_weight         1183.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 112.3730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3288(2)
_cell_length_b                   13.4470(3)
_cell_length_c                   14.5060(3)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.95
_cell_measurement_theta_min      3.03
_cell_volume                     2404.24(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.996
_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       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46544
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.123
_diffrn_reflns_theta_min         3.030
_exptl_absorpt_coefficient_mu    1.624
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.044
_refine_diff_density_min         -1.344
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5298
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0641P)^2^+1.6016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4158
_reflns_number_total             5298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-500-119238.cif
_cod_data_source_block           1210-1
_cod_original_cell_volume        2404.23(8)
_cod_database_code               1565644
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
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
2. Restrained distances
 O9-C20
 1.4 with sigma of 0.002
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C3(H3), C5(H5), C16(H16), C14(H14), C15(H15), C4(H4),
 C9(H9), C20(H20)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C22(H22A,H22B,
 H22C)
;