Transition-metal(ii) complexes with a tripodal hexadentate ligand, 1,1,1-tris[2-aza-3-(imidazol-4-yl)prop-2-enyl]ethane, exhibiting incomplete total or absolute spontaneous resolution
Matsushima, Misaki; Wada, Koki; Horino, Yuki; Takahara, Kazuma; Sunatsuki, Yukinari; Suzuki, Takayoshi; CrystEngComm 22 (2020) 458–466; doi:10.1039/C9CE01864F

data_7239675
_publ_section_title
;
 Transition-metal(ii) complexes with a tripodal hexadentate ligand,
 1,1,1-tris[2-aza-3-(imidazol-4-yl)prop-2-enyl]ethane, exhibiting
 incomplete total or absolute spontaneous resolution
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              458
_journal_page_last               466
_journal_paper_doi               10.1039/C9CE01864F
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         '(C17 H21 Fe N9 2+)2, (Cl O4 1-)4, H2 O'
_chemical_formula_sum            'C34 H44 Cl4 Fe2 N18 O17'
_chemical_formula_weight         1230.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-11-23 deposited with the CCDC.	2019-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                80.2128(17)
_cell_angle_beta                 79.7746(12)
_cell_angle_gamma                80.6301(16)
_cell_formula_units_Z            2
_cell_length_a                   10.2032(3)
_cell_length_b                   12.8833(5)
_cell_length_c                   19.1031(6)
_cell_measurement_reflns_used    36193
_cell_measurement_temperature    192(2)
_cell_measurement_theta_max      30.09
_cell_measurement_theta_min      3.02
_cell_volume                     2412.39(14)
_computing_cell_refinement       'RAPID AUTO (Rigaku, ????)'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO (Rigaku, ????)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      192(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37308
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         3.017
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.8384
_exptl_absorpt_correction_T_min  0.6581
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.999
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         11031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0576
_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^)+(0.1086P)^2^+2.7608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9791
_reflns_number_total             11031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01864f2.cif
_cod_data_source_block           FeH3LClO42
_cod_depositor_comments
;Adding full bibliography for 7239672--7239677.cif.

 Adding full bibliography for 7239672--7239677.cif.
;
_cod_original_cell_volume        2412.38(14)
_cod_database_code               7239675
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.658
_shelx_estimated_absorpt_t_max   0.838
_shelx_res_checksum              37566