Influence of the Synthesis Parameters onto Nucleation and Crystallization of Five New Tin-Sulfur Containing Compounds.
Hilbert, Jessica; Näther, Christian; Bensch, Wolfgang; Inorganic chemistry 53 (2014) 5619–5630; doi:10.1021/ic500369m

data_4338467
_publ_section_title
;
 Influence of the Synthesis Parameters onto Nucleation and Crystallization
 of Five New Tin-Sulfur Containing Compounds.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5619
_journal_page_last               5630
_journal_paper_doi               10.1021/ic500369m
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'Sn2S6, Mn2C48H32N8'
_chemical_formula_sum            'C48 H32 Mn2 N8 S6 Sn2'
_chemical_formula_weight         1260.44
_chemical_name_common            '[Mn(phen)2]2Sn2S6'
_chemical_name_systematic        '[Mn(C12H8N2)2]2Sn2S6'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.356(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.8230(4)
_cell_length_b                   9.8940(2)
_cell_length_c                   24.8107(10)
_cell_measurement_reflns_used    4449
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.62
_cell_measurement_theta_min      1.64
_cell_volume                     2656.05(15)
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_collection       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       '\f 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  0.1060
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28028
_diffrn_reflns_theta_full        24.62
_diffrn_reflns_theta_max         24.62
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.670
_exptl_absorpt_correction_T_max  0.8327
_exptl_absorpt_correction_T_min  0.6774
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.0048(3)
_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   1.120
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+2.4075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                3840
_reflns_number_total             4449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500369m_si_002.cif
_cod_data_source_block           jh231
_cod_depositor_comments
'Adding full bibliography for 4338466--4338470.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4338467