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_7043262
_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_absolute_configuration unk
_chemical_formula_moiety
'C144 H198 Cl11 Cu11 N42, 6(C2 H6 O), 11(Cl), 6(H2O)'
_chemical_formula_sum            'C156 H246 Cl22 Cu11 N42 O12'
_chemical_formula_weight         4380.77
_space_group_crystal_system      cubic
_space_group_IT_number           197
_space_group_name_Hall           'I 2 2 3'
_space_group_name_H-M_alt        'I 2 3'
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_date             2016-07-08T15:13:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_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                90
_cell_formula_units_Z            4
_cell_length_a                   26.85010(10)
_cell_length_b                   26.85010(10)
_cell_length_c                   26.85010(10)
_cell_measurement_reflns_used    30575
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      73.2610
_cell_measurement_theta_min      3.2680
_cell_volume                     19356.99(12)
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5908
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            73532
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.746
_diffrn_reflns_theta_min         3.292
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.599
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9060
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.688
_refine_diff_density_min         -1.806
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     381
_refine_ls_number_reflns         6505
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.09
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0837
_refine_ls_shift/su_max          2.593
_refine_ls_shift/su_mean         0.02
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1878P)^2^+9.7076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2415
_reflns_number_gt                6034
_reflns_number_total             6505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00104e2.cif
_cod_data_source_block           4
_cod_original_cell_volume        19357.0(2)
_cod_database_code               7043262
_publcif_datablock.id            {323cb2f9-b221-40f0-9a7c-3100bf0d038b}