Coordination effects in hydrated manganese(II) 1,3-diethyl-2-thiobarbiturates and their thermal stability
Nicolay N. Golovnev; Maxim S. Molokeev; Irina V. Sterkhova; Maxim K. Lesnikov; Victor V. Atuchin; Polyhedron 134 (2017) 120–125; doi:10.1016/j.poly.2017.06.002

data_1546429
_publ_section_title
;
 Coordination effects in hydrated manganese(II)
 1,3-diethyl-2-thiobarbiturates and their thermal stability
;
_journal_issue                   0
_journal_name_full               Polyhedron
_journal_page_first              120
_journal_page_last               125
_journal_paper_doi               10.1016/j.poly.2017.06.002
_journal_volume                  134
_journal_year                    2017
_chemical_formula_moiety         'C48 H86 Mn3 N12 O22 S6'
_chemical_formula_sum            'C48 H86 Mn3 N12 O22 S6'
_chemical_formula_weight         1540.47
_chemical_name_systematic
;
Bis(mu~2~-1,3-diethyl-2-thiobarbiturato-O,O')-tetrakis(1,3-diethyl-
2-thiobarbiturato-O)-decaaqua-trimanganese(II)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                109.494(3)
_cell_angle_beta                 92.834(3)
_cell_angle_gamma                106.941(3)
_cell_formula_units_Z            1
_cell_length_a                   9.0094(8)
_cell_length_b                   14.0378(11)
_cell_length_c                   14.5823(12)
_cell_measurement_reflns_used    81284
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.195
_cell_measurement_theta_min      2.395
_cell_volume                     1640.9(2)
_computing_cell_refinement       'APEX2 (Bruker, 2003-2008)'
_computing_data_collection       'APEX2 (Bruker, 2003-2008)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0921
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            81284
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.195
_diffrn_reflns_theta_min         2.395
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Bruker, 2004)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       needle
_exptl_crystal_F_000             805
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         9700
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+0.3364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1265
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7088
_reflns_number_total             9700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Mn3H2O10DETBA6.cif
_cod_data_source_block           b
_cod_database_code               1546429
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              18861
_shelx_hkl_checksum              71114