Solvent-Dependent Self-Assembly of an Oxalato-Based Three-Dimensional Magnet Exhibiting a Novel Architecture.
Mon, Marta; Grancha, Thais; Verdaguer, Michel; Train, Cyrille; Armentano, Donatella; Pardo, Emilio; Inorganic chemistry 55 (2016) 6845–6847; doi:10.1021/acs.inorgchem.6b01256

data_4348504
_publ_section_title
;
 Solvent-Dependent Self-Assembly of an Oxalato-Based Three-Dimensional
 Magnet Exhibiting a Novel Architecture.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6845
_journal_page_last               6847
_journal_paper_doi               10.1021/acs.inorgchem.6b01256
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C54 H96 Cr4 Mn3 N6 O54'
_chemical_formula_weight         2066.18
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   26.3296(16)
_cell_length_b                   26.3296(16)
_cell_length_c                   23.314(3)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.3
_cell_measurement_theta_min      2.5
_cell_volume                     13997(2)
_computing_cell_refinement       'Bruker APEX'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.710
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_Laue_measured_fraction_full 0.710
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            70469
_diffrn_reflns_point_group_measured_fraction_full 0.708
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.321
_diffrn_reflns_theta_min         1.547
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             6390
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_coef       0.00012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         3985
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0813P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    0.706
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3765
_reflns_number_total             3985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01256_si_002.cif
_cod_data_source_block           1_SQ
_cod_database_code               4348504
_shelxl_version_number           2013-4
_shelx_res_checksum              83992
_shelx_hkl_checksum              94289