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_7043261
_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         2(ClO4),(O),(C24H30N6Zn)
_chemical_formula_sum            'C24 H30 Cl2 N6 O9 Zn'
_chemical_formula_weight         682.81
_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   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                 100.2980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5454(2)
_cell_length_b                   14.1957(3)
_cell_length_c                   24.2629(6)
_cell_measurement_reflns_used    15340
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.12
_cell_measurement_theta_min      6.51
_cell_volume                     2895.87(12)
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
 scan:  N=1,PHI=270.0,CHI=40.0,OMEGA=5.0,185.0,5.0,COUPLE=0.00                 
 scan:  N=2,PHI=180.0,CHI=40.0,OMEGA=144.0,234.0,5.0,COUPLE=0.00               
 scan:  N=3,PHI=270.0,CHI=15.0,OMEGA=5.0,155.0,5.0,COUPLE=0.00                 
 scan:  N=4,PHI=0.0,CHI=40.0,OMEGA=72.0,117.0,5.0,COUPLE=0.00                  
 scan:  N=5,PHI=0.0,CHI=0.0,OMEGA=20.0,200.0,5.0,COUPLE=0.00                   
 Orientation Matrix:
    UB11  0.0493 UB12 -0.0582 UB13 -0.0126
    UB21 -0.0714 UB22  0.0048 UB23 -0.0373
    UB31  0.0814 UB32  0.0394 UB33 -0.0141
    Matrix type: 'd*Trek'
;
_diffrn_measurement_device_type  RAXIS-RAPID
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       RX
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20821
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        58.920
_diffrn_reflns_theta_max         58.920
_diffrn_reflns_theta_min         6.506
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0000
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    3.415
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5159
_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    1.566
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.070
_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     406
_refine_ls_number_reflns         4076
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+2.9952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1537
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3202
_reflns_number_total             4076
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {d163bc37-05fa-4ff3-b805-2192bb3d9edc}
_cod_data_source_file            c7dt00104e2.cif
_cod_data_source_block           1
_cod_database_code               7043261
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.280
_shelx_estimated_absorpt_t_max   0.848
_exptl_absorpt_special_details
;
 T.Higashi, Empirical Absorption Correction, 2001
;
_shelx_res_checksum              18474