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_7239676
_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_absolute_configuration ad
_chemical_formula_moiety         'C17 H21 N9 Ni 2+, Cl O4 1-, Cl 1-'
_chemical_formula_sum            'C17 H21 Cl2 N9 Ni O4'
_chemical_formula_weight         545.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-12-03 deposited with the CCDC.	2019-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4888(7)
_cell_length_b                   14.7278(9)
_cell_length_c                   15.9298(10)
_cell_measurement_reflns_used    19969
_cell_measurement_temperature    192(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.05
_cell_volume                     2226.2(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.1'
_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 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21638
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.461
_diffrn_reflns_theta_min         3.048
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.150
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 2001 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0228
_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^)+(0.0301P)^2^+0.0674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0553
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                4872
_reflns_number_total             5069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01864f2.cif
_cod_data_source_block           NiH3LClO4Cl
_cod_depositor_comments
;Adding full bibliography for 7239672--7239677.cif.

 Adding full bibliography for 7239672--7239677.cif.
;
_cod_original_cell_volume        2226.2(2)
_cod_database_code               7239676
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.687
_shelx_estimated_absorpt_t_max   0.893
_shelx_res_checksum              65483