Supramolecular Structure of Tris(1,10-phenanthroline)zinc(II)-Cation and N,N′,N″-tris(carboxymethyl)-1,3,5-benzenetricarboxamide-Anion: Synthesis, Crystal Structure, Vibrational Spectra, and Theoretical Investigations
Pook, Niels-Patrick; Crystals 13 (2023) 569–; doi:10.3390/cryst13040569

data_1568782
_publ_section_title
;
 Supramolecular Structure of Tris(1,10-phenanthroline)zinc(II)-Cation and
 N,N&#x2032;,N&#x2033;-tris(carboxymethyl)-1,3,5-benzenetricarboxamide-Anion:
 Synthesis, Crystal Structure, Vibrational Spectra, and Theoretical
 Investigations
;
_journal_issue                   4
_journal_name_full               Crystals
_journal_page_first              569
_journal_paper_doi               10.3390/cryst13040569
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C36 H24 N6 Zn, C15 H13 N3 O9, 5(H2 O)'
_chemical_formula_sum            'C51 H47 N9 O14 Zn'
_chemical_formula_weight         1075.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.6426(7)
_cell_length_b                   20.0946(13)
_cell_length_c                   32.345(2)
_cell_measurement_reflns_used    24712
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      1.66
_cell_volume                     9517.1(10)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      223
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      ' 180 frames, detector distance = 120 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1181
_diffrn_reflns_av_unetI/netI     0.1172
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            28115
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.832
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           30
_diffrn_source_power             1.20
_diffrn_source_voltage           40
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  0.9159
_exptl_absorpt_correction_T_min  0.8040
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Area, X-RED (2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       block
_exptl_crystal_F_000             4464
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         8439
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4396
_reflns_number_total             8439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            C51H47N9O14Zn.cif
_cod_data_source_block           C51H47N9O14Zn
_cod_original_cell_volume        9517.0(10)
_cod_database_code               1568782
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              39030
_shelx_hkl_checksum              22734