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_4338470
_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         'Mn2C48H32N8, Sn2S6, C12H8N2'
_chemical_formula_sum            'C60 H40 Mn2 N10 S6 Sn2'
_chemical_formula_weight         1440.64
_chemical_name_common            '[Mn(phen)2]2Sn2S6_phen'
_chemical_name_systematic
; 
 [Mn(C12H8N2)2]2Sn2S6_C12H8N2 
;
_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                71.700(7)
_cell_angle_beta                 81.458(7)
_cell_angle_gamma                84.346(7)
_cell_formula_units_Z            1
_cell_length_a                   10.0642(9)
_cell_length_b                   10.6249(9)
_cell_length_c                   13.6927(12)
_cell_measurement_reflns_used    11651
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.78
_cell_measurement_theta_min      1.58
_cell_volume                     1372.6(2)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1135
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11651
_diffrn_reflns_theta_full        22.78
_diffrn_reflns_theta_max         22.78
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.629
_exptl_absorpt_correction_T_max  0.8224
_exptl_absorpt_correction_T_min  0.7221
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         11661
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0634
_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^)+(0.0434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1242
_reflns_number_gt                8029
_reflns_number_total             11661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500369m_si_003.cif
_cod_data_source_block           jh607b5
_cod_depositor_comments
'Adding full bibliography for 4338466--4338470.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4338470