Constructing Asymmetrical Ni-Centered {NiN2O4} Octahedra in Layered Metal-Organic Structures for Near-Room-Temperature Single-Phase Magnetoelectricity.
Mao, Kaihui; Zhang, Jinlei; Guo, Zijing; Liu, Lizhe; Ma, He; Chin, Yiying; Lin, Hong-Ji; Bao, Songsong; Xie, Hangqing; Yang, Run; Jing, Zhaoyang; Shen, Jiancang; Yuan, Guoliang; Chen, Jian; Wu, Peiheng; Wu, Xinglong; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c05845

data_4135109
_publ_section_title
;
 Constructing Asymmetrical Ni-Centered {NiN2O4} Octahedra in Layered
 Metal-Organic Structures for Near-Room-Temperature Single-Phase
 Magnetoelectricity.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c05845
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C72 H76 N8 Ni2 O12, 4(H2 O)'
_chemical_formula_sum            'C72 H84 N8 Ni2 O16'
_chemical_formula_weight         1434.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 117.280(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.205(8)
_cell_length_b                   23.187(8)
_cell_length_c                   16.965(5)
_cell_measurement_reflns_used    6223
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.602
_cell_measurement_theta_min      2.512
_cell_volume                     8113(5)
_computing_cell_refinement       'APEX 3'
_computing_data_collection       'APEX 3'
_computing_data_reduction        'APEX 3'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.1449
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24876
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.512
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_crystal_colour            'bluish green'
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       sheet-like
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.367
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         14737
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1503
_refine_ls_R_factor_gt           0.0817
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+45.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1938
_refine_ls_wR_factor_ref         0.2375
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    0.845
_reflns_Friedel_fraction_max     0.845
_reflns_number_gt                8567
_reflns_number_total             14737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c05845_si_003.cif
_cod_data_source_block           c2-173k
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4135109
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.902
_shelx_estimated_absorpt_t_max   0.990
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              91378
_shelx_hkl_checksum              10021
_shelx_fab_checksum              37094