Polar Ferromagnetic Metal by Intercalation of Metal‒Amine Complexes
Zheng, Huafei; Wilfong, Brandon C.; Hickox-Young, Daniel; Rondinelli, James M.; Zavalij, Peter Y.; Rodriguez, Efrain E.; Chemistry of Materials  (2021) –; doi:10.1021/acs.chemmater.1c00540

data_4003966
_publ_section_title
;
 Polar Ferromagnetic Metal by Intercalation of Metal--Amine Complexes
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.1c00540
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Co12 S12, C6 H24 Co N6, C2 H8 N2'
_chemical_formula_sum            'C8 H32 Co13 N8 S12'
_chemical_formula_weight         1391.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.778(3)
_cell_length_b                   11.066(3)
_cell_length_c                   20.095(5)
_cell_measurement_reflns_used    1808
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      2.5
_cell_volume                     3286.2(14)
_computing_cell_refinement       'Apex2, Saint (Bruker, 2012)'
_computing_data_collection       'Apex2 (Bruker, 2012)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'Olex2 (Dolomanov, 2009)'
_computing_publication_material  'Apex2, SHELXL, Platon (Spek, 2015)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015c)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0321630
_diffrn_orient_matrix_UB_12      0.0632584
_diffrn_orient_matrix_UB_13      0.0003160
_diffrn_orient_matrix_UB_21      -0.0109193
_diffrn_orient_matrix_UB_22      -0.0036757
_diffrn_orient_matrix_UB_23      0.0493348
_diffrn_orient_matrix_UB_31      0.0837580
_diffrn_orient_matrix_UB_32      0.0237882
_diffrn_orient_matrix_UB_33      0.0065945
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34881
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.490
_diffrn_reflns_theta_min         1.840
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    7.155
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.453
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Krause et al, 2015)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.812
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2716
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.007
_refine_diff_density_max         1.927
_refine_diff_density_min         -1.293
_refine_diff_density_rms         0.231
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         6804
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1610
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0960P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.2249
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2756
_reflns_number_total             6804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm1c00540_si_002.cif
_cod_data_source_block           UM3418
_cod_original_cell_volume        3286.3(13)
_cod_database_code               4003966
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.434
_shelx_estimated_absorpt_t_max   0.965
_shelx_res_checksum              22151
_shelx_hkl_checksum              37349