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_7043740
_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_formula_moiety         'C48 H30 N19 Ni2 O13 Tb, 4(O), C4 H8 O'
_chemical_formula_sum            'C52 H53 N19 Ni2 O17.5 Tb'
_chemical_formula_weight         1500.47
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-05-23 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.977(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2817(6)
_cell_length_b                   24.8997(8)
_cell_length_c                   20.7090(8)
_cell_measurement_reflns_used    15039
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.7047
_cell_measurement_theta_min      2.9421
_cell_volume                     6514.3(5)
_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_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  Xcalibur
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.1398
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            66009
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.800
_diffrn_reflns_theta_min         2.943
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.82835
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3036
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.237
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     890
_refine_ls_number_reflns         20407
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1427
_refine_ls_R_factor_gt           0.0643
_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^)+(0.1005P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10292
_reflns_number_total             20407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02288c2.cif
_cod_data_source_block           dc170_CCDC1
_cod_original_formula_sum        'C52 H53 N19 Ni2 O17.50 Tb'
_cod_database_code               7043740
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C50-C49 = C51-C50 = C52-C51
 1.5 with sigma of 0.02
 O14-C49 = O14-C52
 1.35 with sigma of 0.02
 N14-C19 \\sim N14-C18A
 with sigma of 0.02
 C20-C19 \\sim C18A-C17 \\sim C18-C17
 with sigma of 0.02
 O3-C21 \\sim O3A-C21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3A) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C20A)
\\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(N14A) \\sim Ueq, Uanis(C18A) \\sim Ueq,
Uanis(C17A) \\sim Ueq, Uanis(N3A) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Sof(O3A)=Sof(N3A)=Sof(N14A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=
 Sof(H19A)=Sof(C20A)=Sof(C21A)=Sof(O16A)=1-FVAR(1)
 Sof(O3)=Sof(N3)=Sof(N14)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=
 Sof(H19)=Sof(C20)=Sof(C21)=Sof(O16)=FVAR(1)
 Sof(O19A)=1-FVAR(2)
 Sof(O19)=FVAR(2)
 Fixed Sof: O14(0.5) C49(0.5) H49a(0.5) H49b(0.5) C50(0.5) H50a(0.5) H50b(0.5)
 C51(0.5) H51a(0.5) H51b(0.5) C52(0.5) H52a(0.5) H52b(0.5) O18(0.5) O15(0.5)
 C53(0.5) H53a(0.5) H53b(0.5) C54(0.5) H54a(0.5) H54b(0.5) C55(0.5) H55a(0.5)
 H55b(0.5) C56(0.5) H56a(0.5) H56b(0.5) O20(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C49(H49a,H49b), C50(H50a,H50b), C51(H51a,H51b), C52(H52a,H52b), C53(H53a,
 H53b), C54(H54a,H54b), C55(H55a,H55b), C56(H56a,H56b)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C11(H11), C14(H14), C15(H15),
 C16(H16), C17(H17), C17A(H17A), C18(H18), C18A(H18A), C19(H19), C19A(H19A),
 C23(H23), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C35(H35), C39(H39), C40(H40), C41(H41), C43(H43), C46(H46),
 C47(H47), C48(H48)
;
_shelx_res_checksum              6138
_olex2_submission_special_instructions 'No special instructions were received'