Synthesis, Crystal Structure, and High-Precision High-Frequency and -Field Electron Paramagnetic Resonance Investigation of a Manganese(III) Complex: [Mn(dbm)2(py)2](ClO4)
Aromí, Guillem; Telser, Joshua; Ozarowski, Andrew; Brunel, Louis-Claude; Stoeckli-Evans, Helen-Margaret; Krzystek, J.; Inorganic Chemistry 44 (2005) 187–196; doi:10.1021/ic049180u

data_4308420
_publ_section_title
;
 Synthesis, Crystal Structure, and High-Precision High-Frequency and -Field
 Electron Paramagnetic Resonance Investigation of a Manganese(III) Complex:
 [Mn(dbm)2(py)2](ClO4)
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              187
_journal_page_last               196
_journal_paper_doi               10.1021/ic049180u
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C40 H32 Mn N2 O4, (Cl O4)'
_chemical_formula_sum            'C40 H32 Cl Mn N2 O8'
_chemical_formula_weight         759.07
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.144(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2851(4)
_cell_length_b                   24.0826(9)
_cell_length_c                   17.9576(9)
_cell_measurement_reflns_used    48862
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.595
_cell_measurement_theta_min      1.615
_cell_volume                     3527.0(3)
_computing_cell_refinement       'X-Area V1.17 (STOE & Cie GmbH, 2002)'
_computing_data_collection       'X-Area V1.17 (STOE & Cie GmbH, 2002)'
_computing_data_reduction        'X-RED32 V1.04 (STOE & Cie GmbH, 2002)'
_computing_molecular_graphics    'PLATON99 (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'rotation method'
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46621
_diffrn_reflns_theta_full        29.51
_diffrn_reflns_theta_max         29.51
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0036(6)
_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   1.141
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         9792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+1.0294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                8317
_reflns_number_total             9792
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic049180usi20040623_114341.cif
_cod_data_source_block           ga-mndbm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4308420