Synthetic ability of dinuclear mesocates containing 1,3-bis(diazinecarboxamide)benzene bridging ligands to form complexes of increased nuclearity. Crystal structures, magnetic properties and theoretical studies.
Palacios, Maria A.; Morlieras, Jessica; Herrera, Juan Manuel; Mota, Antonio J.; Brechin, Euan K.; Triki, Smail; Colacio, Enrique; Dalton Trans.  (2017) –; doi:10.1039/C7DT02288C

data_7043735
_publ_section_title
;
 Synthetic ability of dinuclear mesocates containing
 1,3-bis(diazinecarboxamide)benzene bridging ligands to form complexes of
 increased nuclearity. Crystal structures, magnetic properties and
 theoretical studies.
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02288C
_journal_year                    2017
_chemical_compound_source        'Maria Angeles Palacios Lopez'
_chemical_formula_moiety         'C132 H114 Mn3 N42 Ni4 O18, 2(C24 H20 P)'
_chemical_formula_sum            'C180 H144 Mn3 N42 Ni4 O18 P2'
_chemical_formula_weight         3644.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc1jd6mr
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-09 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                92.0192(16)
_cell_angle_beta                 98.6580(17)
_cell_angle_gamma                104.5213(16)
_cell_formula_units_Z            2
_cell_length_a                   18.9329(4)
_cell_length_b                   20.4784(4)
_cell_length_c                   25.2751(5)
_cell_measurement_reflns_used    23186
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.2796
_cell_measurement_theta_min      2.2333
_cell_volume                     9351.1(3)
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Shelxs Sheldrick'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega -112.00  -14.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164  -37.0000   90.0000 98

  2 omega -109.00  -14.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164  -37.0000    0.0000 95

  3 omega -121.00  -55.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164 -164.0000  109.0000 66

  4 omega  -82.00  -54.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164 -164.0000 -134.0000 28

  5 omega   60.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3164  179.0000   30.0000 60

  6 omega   86.00  130.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3164  179.0000 -180.0000 44

  7 omega   68.00   95.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  164.0000 -109.0000 27

  8 omega   32.00   66.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  -45.0000 -120.0000 34

  9 omega   32.00   67.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  -45.0000  -90.0000 35

 10 omega   32.00   76.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  -45.0000    0.0000 44

 11 omega   43.00   70.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  -45.0000  -60.0000 27

 12 omega  101.00  164.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  125.0000 -150.0000 63

 13 omega   80.00  119.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667   45.0000 -180.0000 39

 14 omega   95.00  139.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667 -164.0000   45.0000 44

 15 omega   39.00   67.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667 -116.0000 -102.0000 28

 16 omega  134.00  161.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  164.0000 -109.0000 27

 17 omega   88.00  115.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667 -116.0000 -102.0000 27

 18 omega   80.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667   45.0000    0.0000 62

 19 omega  143.00  168.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  125.0000   30.0000 25

 20 omega   83.00  162.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667   45.0000 -150.0000 79

 21 omega   29.00  138.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  -77.0000  120.0000 109

 22 omega   81.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667   45.0000  -90.0000 97

 23 omega   30.00  113.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667 -110.0000   47.0000 83

 24 omega  -67.00   36.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164   37.0000 -180.0000 103

 25 omega -129.00  -34.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164  179.0000 -180.0000 95

 26 omega -119.00   -7.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164  -77.0000  -90.0000 112

 27 omega -119.00   -7.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164  -77.0000    0.0000 112

 28 omega    7.00  119.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3164   77.0000 -180.0000 112

 29 omega   68.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3164  164.0000  134.0000 52

 30 omega   46.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667   15.0000  120.0000 132

 31 omega   74.00  111.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667   77.0000  -60.0000 37

;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            106563
_diffrn_reflns_theta_full        67.68
_diffrn_reflns_theta_max         73.44
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    2.772
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
(compiled Dec  8 2009,17:31:18)
Analytical numeric absorption correction using a multifaceted crystal
    model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             3758
_exptl_crystal_size_max          0.1695
_exptl_crystal_size_mid          0.1164
_exptl_crystal_size_min          0.0895
_platon_squeeze_details
;
;
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.709
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1807
_refine_ls_number_reflns         36654
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      0.712
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1650
_reflns_number_gt                22953
_reflns_number_total             36654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt02288c2.cif
_cod_data_source_block           eb0029
_cod_original_cell_volume        9351.0(3)
_cod_database_code               7043735