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_1565643
_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         'C21 H26 Co2 N2 O10'
_chemical_formula_sum            'C21 H26 Co2 N2 O10'
_chemical_formula_weight         584.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                75.073(5)
_cell_angle_beta                 86.887(4)
_cell_angle_gamma                68.260(5)
_cell_formula_units_Z            2
_cell_length_a                   9.9509(4)
_cell_length_b                   10.7756(6)
_cell_length_c                   12.2089(7)
_cell_measurement_reflns_used    3145
_cell_measurement_temperature    292.90(10)
_cell_measurement_theta_max      28.3130
_cell_measurement_theta_min      3.8440
_cell_volume                     1173.74(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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 (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.90(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    1.00   27.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   57.0000   60.0000 26

  2 omega    6.00   41.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   57.0000  -90.0000 35

  3 omega  -41.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -57.0000  -90.0000 87

  4 omega  -10.00   23.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4273  -99.0000  -60.0000 33

  5 omega  -48.00   32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -57.0000  150.0000 80

  6 omega  -50.00   56.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -77.0000   60.0000 106

  7 omega   77.00  102.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  178.0000  -90.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0049849000
_diffrn_orient_matrix_UB_12      0.0697345000
_diffrn_orient_matrix_UB_13      -0.0161411000
_diffrn_orient_matrix_UB_21      0.0311702000
_diffrn_orient_matrix_UB_22      -0.0097361000
_diffrn_orient_matrix_UB_23      -0.0522551000
_diffrn_orient_matrix_UB_31      -0.0700335000
_diffrn_orient_matrix_UB_32      0.0204068000
_diffrn_orient_matrix_UB_33      -0.0251313000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7721
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4616
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.7116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                3853
_reflns_number_total             4616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2020-500-119238.cif
_cod_data_source_block           w355co
_cod_original_cell_volume        1173.74(11)
_cod_database_code               1565643
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H) groups
2. Restrained distances
 O9-H9
 0.85 with sigma of 0.01
 O10-H10
 0.85 with sigma of 0.01
 C18-H9
 1.899793 with sigma of 0.02
 Co2-H9
 2.854413 with sigma of 0.02
 C19-H10
 1.884036 with sigma of 0.02
 Co2-H10
 2.805748 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C10(H10A), C12(H12), C13(H13), C14(H14)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C)
;