Syntheses, Crystal Structures, and Spectroscopic and Magnetic Properties of [Mn2III(H2L1)(Cl4Cat)4.2H2O]∞and [Mn2III(H2L2)(Cl4Cat)4.2CH3CN.2H2O]\ιnfty: Temperature-Dependent Valence Tautomerism in Solution
Nizamuddin Shaikh; Sanchita Goswami; Anangamohan Panja; Hao-Ling Sun; Feng Pan; Song Gao; Pradyot Banerjee; Inorganic Chemistry 44 (2005) 9714–9722; doi:10.1021/ic051064j

data_4310216
_publ_section_title
;
Syntheses, Crystal Structures, and Spectroscopic and Magnetic Properties of
[Mn2III(H2L1)(Cl4Cat)4.2H2O]\\infty and
[Mn2III(H2L2)(Cl4Cat)4.2CH3CN.2H2O]\\infty: Temperature-Dependent Valence
Tautomerism in Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9714
_journal_page_last               9722
_journal_paper_doi               10.1021/ic051064j
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C38 H22 Cl16 Mn2 N4 O10'
_chemical_formula_weight         1371.68
_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                116.100(2)
_cell_angle_beta                 96.9030(10)
_cell_angle_gamma                100.861(2)
_cell_formula_units_Z            1
_cell_length_a                   9.1408(3)
_cell_length_b                   12.0072(4)
_cell_length_c                   12.7159(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1197.79(8)
_computing_cell_refinement       'Rapid auto Rigaku 2001'
_computing_data_collection       'Rapid auto Rigaku 2001'
_computing_data_reduction        'Rapid auto Rigaku 2001'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_measured_fraction_theta_full 0.705
_diffrn_measured_fraction_theta_max 0.705
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.0807
_diffrn_reflns_av_sigmaI/netI    0.1461
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4757
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    1.481
_exptl_absorpt_correction_T_max  0.9296
_exptl_absorpt_correction_T_min  0.6328
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
                                  HIGASHI, T. (1995). Abscor-Empirical
                                  Absorption
                                  Correction based on Fourier Series
                                  Approximation.Rigaku Corporation,Tokyo,
                                  Japan.
;
_exptl_crystal_colour            needle
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       green
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.2218
_refine_ls_R_factor_gt           0.1071
_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^)+(0.1793P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2550
_refine_ls_wR_factor_ref         0.3179
_reflns_number_gt                1489
_reflns_number_total             3880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051064jsi20050628_061941.cif
_cod_data_source_block           sx148
_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.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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 
;
_cod_original_cell_volume        1197.79(7)
_cod_database_code               4310216