Field-Induced Slow Relaxation in a Monometallic Manganese(III) Single-Molecule Magnet.
Craig, Gavin A.; Marbey, Jonathan J.; Hill, Stephen; Roubeau, Olivier; Parsons, Simon; Murrie, Mark; Inorganic chemistry 54 (2015) 13–15; doi:10.1021/ic5024136

data_4341904
_publ_section_title
;
 Field-Induced Slow Relaxation in a Monometallic Manganese(III)
 Single-Molecule Magnet.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              13
_journal_page_last               15
_journal_paper_doi               10.1021/ic5024136
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 H24 Mn1 Na5 O22, 2(H2 O)'
_chemical_formula_sum            'C8 H28 Mn Na5 O24'
_chemical_formula_weight         678.17
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2014-09-28
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                90
_cell_angle_beta                 112.375(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.103(5)
_cell_length_b                   6.7980(13)
_cell_length_c                   9.611(2)
_cell_measurement_reflns_used    2536
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      2.19
_cell_volume                     1214.6(5)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.080
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10148
_diffrn_reflns_theta_full        25.688
_diffrn_reflns_theta_max         25.688
_diffrn_reflns_theta_min         2.191
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.25
_refine_ls_abs_structure_details 'Flack (1983), 1050 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9465
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         2312
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.0042831
_refine_ls_shift/su_mean         0.0002208
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 0.18P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0764
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0764
_reflns_limit_h_max              22
_reflns_limit_h_min              -24
_reflns_limit_k_max              8
_reflns_limit_k_min              -8
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                2127
_reflns_number_total             2314
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0393
_oxford_refine_ls_scale          0.14843(8)
_oxford_reflns_number_all        2312
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'GAC233 in C2'
_cod_data_source_file            ic5024136_si_002.cif
_cod_data_source_block           gac233
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4341904.cif.
;
_cod_original_cell_volume        1214.5(5)
_cod_original_sg_symbol_H-M      'C 2 '
_cod_original_formula_sum        'C8 H28 Mn1 Na5 O24'
_cod_database_code               4341904
_iucr_refine_instructions_details_constraints
;
BLOCK 
CONT SCALE 
CONT MN   (    1 ,X'S,U'S)  UNTIL O    (    6 ) 
CONT H    (   10 ,X'S,U[ISO])  UNTIL H    (   62 ) 
CONT ENANTIO 
END                                                                             
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_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM NO H   NO #H U MULT DIST 
REM C-H 
REM >4           1.5    .96 DISORDER 
REM 1      1     1.2    .93 C C-H (ACETYLENE) 
REM 1      2     1.2    .93 C-C(H)-C 
REM 1      3     1.2    .98 (C)3-C-H 
REM 2      1     1.2    .93 C=C-H(2) 
REM 2      2     1.2    .97 (C)2-C-(H)2 
REM 3      1     1.5    .96 C-C-(H)3 
REM N-H 
REM >4           1.5    .89 DISORDER 
REM 1      1     1.2    .86 N-N/H 
REM 1      2     1.2    .86 (C)2-N-H 
REM 1      3     1.2    .89 (C)3-N-H 
REM 2      1     1.2    .86 C-N-(H)2 
REM 2      2     1.2    .89 (C)2-N-(H)2 
REM 3      1     1.2    .89 C-H-(H)3 
REM O-H 
REM 1      1     1.5    .82 O-H 
REM 
REM DIST      ESD = 0.02 
REM VIB       ESD = 0.002 
REM ANGLE     ESD = 2.0 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 2) TO H(21) 
REST 0.010, 0.002 = H(21,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(21) TO C ( 2) TO C(1,2,1,1) 
CONT H(21) TO C ( 2) TO O(21) 
CONT H(21) TO C ( 2) TO C(3) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 3) TO H(31) 
REST 0.011, 0.002 = H(31,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(31) TO C ( 3) TO C(2) 
CONT H(31) TO C ( 3) TO O(31) 
CONT H(31) TO C ( 3) TO C(4) 
REM       H ON O-HETRO ATOM 
DIST 0.82, 0.02 = 
CONT O ( 1) TO H(10) 
CONT O ( 1) TO H(11) 
REST 0.031, 0.002 = H(10,U[ISO]) 
REST 0.031, 0.002 = H(11,U[ISO]) 
REM       H ON O-HETRO ATOM 
DIST 0.82, 0.02 = 
CONT O ( 2) TO H(20) 
CONT O ( 2) TO H(22) 
REST 0.018, 0.002 = H(20,U[ISO]) 
REST 0.018, 0.002 = H(22,U[ISO]) 
REM       H ON O-HETRO ATOM 
DIST 0.82, 0.02 = 
CONT O ( 3) TO H(32) 
CONT O ( 3) TO H(33) 
REST 0.024, 0.002 = H(32,U[ISO]) 
REST 0.024, 0.002 = H(33,U[ISO]) 
REM       H ON O-HETRO ATOM 
DIST 0.82, 0.02 = 
CONT O ( 4) TO H(41) 
CONT O ( 4) TO H(42) 
REST 0.021, 0.002 = H(41,U[ISO]) 
REST 0.021, 0.002 = H(42,U[ISO]) 
REM       H ON O-HETRO ATOM 
DIST 0.82, 0.02 = 
CONT O ( 5) TO H(51) 
CONT O ( 5) TO H(52) 
REST 0.020, 0.002 = H(51,U[ISO]) 
REST 0.020, 0.002 = H(52,U[ISO]) 
REM       H ON O-HETRO ATOM 
DIST 0.82, 0.02 = 
CONT O ( 6) TO H(61) 
CONT O ( 6) TO H(62) 
REST 0.024, 0.002 = H(61,U[ISO]) 
REST 0.024, 0.002 = H(62,U[ISO]) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 0.820000 , 0.010000 = O(5) TO H(52) 
END                                                                             
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