Metal complexes of ditopic dithiophosphonate ligands built on a naphthalenediimide core
Radu F. Semeniuc; Robert R. Baum; Jedidiah J. Veach; Kraig A. Wheeler; Perry J. Pellechia; Inorganica Chimica Acta 400 (2013) 228–238; doi:

data_1516950
_publ_section_title
;
 Metal complexes of ditopic dithiophosphonate ligands built on a
 naphthalenediimide core
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              228
_journal_page_last               238
_journal_volume                  400
_journal_year                    2013
_chemical_formula_moiety         'C68 H56 N2 O8 P2 S4 Sn2'
_chemical_formula_sum            'C68 H56 N2 O8 P2 S4 Sn2'
_chemical_formula_weight         1456.79
_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
_cell_angle_alpha                75.808(5)
_cell_angle_beta                 78.661(5)
_cell_angle_gamma                87.864(5)
_cell_formula_units_Z            1
_cell_length_a                   9.1471(11)
_cell_length_b                   13.3620(15)
_cell_length_c                   14.7072(17)
_cell_measurement_reflns_used    4575
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.743
_cell_measurement_theta_min      3.159
_cell_volume                     1708.6(3)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction
;
SAINT (Bruker, 2008) and XPREP (Bruker, 2008)
;
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1704
_diffrn_reflns_av_sigmaI/netI    0.1447
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16357
_diffrn_reflns_theta_full        51.72
_diffrn_reflns_theta_max         51.72
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    7.829
_exptl_absorpt_correction_T_max  0.262
_exptl_absorpt_correction_T_min  0.046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2010)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent plate'
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.144
_refine_diff_density_max         1.510
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         3652
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.0990
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1448P)^2^+3.2933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2289
_refine_ls_wR_factor_ref         0.2505
_reflns_number_gt                2417
_reflns_number_total             3652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-400-228-238-1.cif
_cod_data_source_block           2a-[SnPh3]2
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_sg_symbol_H-M      'p -1'
_cod_database_code               1516950