Tailoring the local environment around metal ions: solution chemical and structural study of some multidentate tripodal ligands
Matyuska, Ferenc; Szorcsik, Attila; Nagy, Nora V.; Dancs, Ágnes; Kováts, Éva; Benyei, Attila; Gajda, Tamás; Dalton Trans.  (2017) –; doi:10.1039/C7DT00104E

data_7043259
_publ_section_title
;
 Tailoring the local environment around metal ions: solution chemical and
 structural study of some multidentate tripodal ligands
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00104E
_journal_year                    2017
_chemical_formula_moiety         (C24H30N6Zn),(Cl),(ClO4)
_chemical_formula_sum            'C24 H30 Cl2 N6 O4 Zn'
_chemical_formula_weight         602.81
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-08 deposited with the CCDC.
2017-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   13.9000(5)
_cell_length_b                   13.9000(5)
_cell_length_c                   45.0290(14)
_cell_measurement_reflns_used    44094
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      3.23
_cell_volume                     7534.5(4)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'Spek, A.L. (2003). J.Appl.Cryst. 36,7-13.'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
 scan:  N=1,PHI=180.0,CHI=0.0,OMEGA=20.0,200.0,5.0,COUPLE=0.00                 
 scan:  N=2,PHI=0.0,CHI=0.0,OMEGA=20.0,200.0,5.0,COUPLE=0.00                   
 scan:  N=3,PHI=90.0,CHI=40.0,OMEGA=20.0,200.0,5.0,COUPLE=0.00                 
 scan:  N=4,PHI=180.0,CHI=40.0,OMEGA=20.0,200.0,5.0,COUPLE=0.00                
 Orientation Matrix:
    UB11  0.0687 UB12  0.0153 UB13  0.0110
    UB21  0.0415 UB22  0.0747 UB23 -0.0096
    UB31 -0.0214 UB32  0.0329 UB33  0.0167
    Matrix type: 'd*Trek'
;
_diffrn_measurement_device       RAXIS-RAPID
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       RX
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0093
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            72365
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         3.230
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0000
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear SM 1.4.0 (Rigaku/MSC Inc., 2008).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       chunk
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.711
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0531
_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^)+(0.1034P)^2^+20.5149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.1812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1614
_reflns_number_total             1924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00104e2.cif
_cod_data_source_block           2
_cod_original_cell_volume        7534.5(6)
_cod_database_code               7043259
_publcif_datablock.id            {69e981f3-9788-4bad-9c83-fc473afe6f90}
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.748
_shelx_estimated_absorpt_t_max   0.790
_shelx_res_checksum              603