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_7043736
_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         'C32 H24 Cu2 N12 O6, 2(H2 O)'
_chemical_formula_sum            'C32 H28 Cu2 N12 O8'
_chemical_formula_weight         835.74
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-17 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                116.889(5)
_cell_angle_beta                 100.695(5)
_cell_angle_gamma                101.227(5)
_cell_formula_units_Z            1
_cell_length_a                   7.6178(19)
_cell_length_b                   11.658(3)
_cell_length_c                   11.819(3)
_cell_measurement_reflns_used    16527
_cell_measurement_temperature    100
_cell_measurement_theta_max      40.522
_cell_measurement_theta_min      5.907
_cell_volume                     872.2(4)
_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      100.0
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.1197
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5403
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.051
_diffrn_reflns_theta_min         2.034
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.361400
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SAD V2.05 (?, 2016) was used for absorption correction.
R(int) was 0.0581 before and 0.0282 after correction.
The Ratio of minimum to maximum transmission is 0.3614.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       plate
_exptl_crystal_F_000             426
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.662
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.133
_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     260
_refine_ls_number_reflns         3682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0807
_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^)+(0.1068P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2292
_reflns_number_total             3682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02288c2.cif
_cod_data_source_block           hastalli
_cod_database_code               7043736
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O2W(0.5) H2WA(0.5) H2WB(0.5) O1W(0.5) H1WA(0.5) H1WB(0.5)
3.a Free rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Rotating group:
 O1(H1A,H1B)
3.c 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)
;
_shelx_res_checksum              36594
_olex2_submission_special_instructions 'No special instructions were received'