Synthesis and magnetic property of a cobalt complex constructed by a linear Co‒NNN‒Co unit
Wang, Min-Min; Wang, Chun; Wang, Miao; Wang, Jin; Zhu, Jin-Li; Hu, Lan-Ping; Sun, Tong-Ming; Tang, Yan-Feng; Inorganica Chimica Acta 511 (2020) 119804–; doi:10.1016/j.ica.2020.119804

data_1564165
_publ_section_title
;
 Synthesis and magnetic property of a cobalt complex constructed by a
 linear Co--NNN--Co unit
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119804
_journal_paper_doi               10.1016/j.ica.2020.119804
_journal_volume                  511
_journal_year                    2020
_chemical_formula_moiety         'C64 H64 Co2 N19 O2'
_chemical_formula_sum            'C67 H90 Cl3 Co2 N19 O10'
_chemical_formula_weight         1545.78
_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_Hall           '-P 4 2n'
_space_group_name_H-M_alt        'P 4/m n c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0083(6)
_cell_length_b                   16.0083(6)
_cell_length_c                   29.6119(11)
_cell_measurement_reflns_used    1091
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      50.6670
_cell_measurement_theta_min      3.1240
_cell_volume                     7588.5(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0855
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   14.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       34.3979   57.0000   60.0000 89

  2 omega   70.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   61.0000  -60.0000 88

  3 omega   86.00  160.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  111.0000 -120.0000 74

  4 omega   69.00  151.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   61.0000  -30.0000 82

  5 omega   32.00   83.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -94.0000    0.0000 51
;
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0052589000
_diffrn_orient_matrix_UB_12      -0.0175590000
_diffrn_orient_matrix_UB_13      -0.0511011000
_diffrn_orient_matrix_UB_21      0.0862209000
_diffrn_orient_matrix_UB_22      0.0407813000
_diffrn_orient_matrix_UB_23      -0.0066961000
_diffrn_orient_matrix_UB_31      0.0423648000
_diffrn_orient_matrix_UB_32      -0.0853634000
_diffrn_orient_matrix_UB_33      0.0072574000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            12749
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        59.999
_diffrn_reflns_theta_max         59.999
_diffrn_reflns_theta_min         3.138
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.951
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0802
_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^)+(0.1123P)^2^+4.3702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2172
_refine_ls_wR_factor_ref         0.2487
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1593
_reflns_number_total             2875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-511-119804.cif
_cod_data_source_block           Co2
_cod_original_cell_volume        7588.5(6)
_cod_database_code               1564165
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.441
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     62.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N5) = Uanis(N4) = Uanis(N3)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              25419
_shelx_hkl_checksum              84853
_shelx_fab_checksum              75485