Synthesis, Magnetism, and High-Frequency EPR Spectroscopy of a Family of Mixed-Valent Cuboctahedral Mn13 Complexes with 1,8-Naphthalenedicarboxylate Ligands
Christos Lampropoulos; Changhyun Koo; Stephen O. Hill; Khalil Abboud; George Christou; Inorganic Chemistry 47 (2008) 11180–11190; doi:10.1021/ic801484g

data_4306660
_publ_section_title
;
Synthesis, Magnetism, and High-Frequency EPR Spectroscopy of a Family of
Mixed-Valent Cuboctahedral Mn13 Complexes with 1,8-Naphthalenedicarboxylate
Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11180
_journal_page_last               11190
_journal_paper_doi               10.1021/ic801484g
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C110 H120 Mn13 N13 O51'
_chemical_formula_weight         3144.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.456(1)
_cell_angle_beta                 85.032(1)
_cell_angle_gamma                86.978(1)
_cell_formula_units_Z            3
_cell_length_a                   17.1761(10)
_cell_length_b                   22.9617(14)
_cell_length_c                   24.9168(15)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     9427.5(10)
_computing_cell_refinement
'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)'
_computing_data_collection       'Bruker SMART v5.624 (Bruker 1998)'
_computing_data_reduction        'Bruker SHELXTL v6.12 (Bruker 2000)'
_computing_molecular_graphics    'Bruker SHELXTL v6.12'
_computing_publication_material  'Bruker SHELXTL v6.12'
_computing_structure_refinement  'Bruker SHELXTL v6.12'
_computing_structure_solution    'Bruker SHELXTL v6.12'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1023
_diffrn_reflns_av_sigmaI/netI    0.3085
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            62510
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         0.92
_diffrn_standards_decay_%        '< 1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.352
_exptl_absorpt_correction_T_max  0.9463
_exptl_absorpt_correction_T_min  0.8456
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.12 (Bruker 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plates
_exptl_crystal_F_000             4797
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.700
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1666
_refine_ls_number_reflns         41405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.700
_refine_ls_R_factor_all          0.1664
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0648P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1718
_reflns_number_gt                13087
_reflns_number_total             41405
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic801484g_si_002_1.cif
_cod_data_source_block           xl08
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

2021-04-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C330 H360 Mn39 N38 O152'
_cod_original_formula_weight         9433.22
_cod_original_formula_units_Z            1
_cod_database_code               4306660