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_7043733
_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 H40 N18 Ni2 O11 Tb, C H F3 O3 S, 0.5(H2 O), C4 H8 O'
_chemical_formula_sum            'C53 H50 F3 N18 Ni2 O15.5 S Tb'
_chemical_formula_weight         1552.51
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-23
_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                 101.021(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.001(5)
_cell_length_b                   28.854(5)
_cell_length_c                   18.858(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5876(3)
_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 0.391
_diffrn_measured_fraction_theta_max 0.689
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.391
_diffrn_reflns_Laue_measured_fraction_max 0.689
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16124
_diffrn_reflns_point_group_measured_fraction_full 0.391
_diffrn_reflns_point_group_measured_fraction_max 0.689
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.689
_diffrn_reflns_theta_min         2.824
_exptl_absorpt_coefficient_mu    1.955
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_F_000             3128
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         4159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          2.039
_refine_ls_shift/su_mean         0.036
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0837P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2999
_reflns_number_total             4159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02288c2.cif
_cod_data_source_block           8
_cod_original_formula_sum        'C53 H50 F3 N18 Ni2 O15.50 S Tb'
_cod_database_code               7043733
_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
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O12(0.5) H12A(0.5) H12B(0.5)
3.a Free rotating group:
 O12(H12A,H12B)
3.b Rotating group:
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B), O10(H10A,H10B), O11(H11A,H11B)
3.c Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B)
3.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26),
  C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C39(H39),
 C40(H40), C41(H41), C42(H42), C46(H46), C47(H47), C48(H48)
3.e Idealised tetrahedral OH refined as rotating group:
 O13(H13)
;
_shelx_res_checksum              86004
_olex2_submission_special_instructions 'No special instructions were received'