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_7043739
_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, 8(H2 O)'
_chemical_formula_sum            'C32 H40 Cu2 N12 O14'
_chemical_formula_weight         943.84
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 99.617(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.397(6)
_cell_length_b                   11.832(3)
_cell_length_c                   15.242(4)
_cell_measurement_reflns_used    16563
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      48.786
_cell_measurement_theta_min      4.610
_cell_volume                     4160.2(19)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      273.15
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0904
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11145
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.110
_diffrn_reflns_theta_min         1.766
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.664925
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   empirical
_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    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.419
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0749
_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^)+(0.0553P)^2^+45.8711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.1861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2588
_reflns_number_total             3689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02288c2.cif
_cod_data_source_block           j32_csm
_cod_original_cell_volume        4160.3(18)
_cod_database_code               7043739
_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,H) groups
2.a Free rotating group:
 O1(H1A,H1B), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O1W(H1WA,H1WB), O4W(H4WA,H4WB)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C16(H16), C15(H15), C14(H14), C10(H10), C9(H9)
;
_shelx_res_checksum              71540
_olex2_submission_special_instructions 'No special instructions were received'