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_1516951
_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         'C104 H86 Cu2 N2 O8 P6 S4, 2(C H2 Cl2)'
_chemical_formula_sum            'C106 H90 Cl4 Cu2 N2 O8 P6 S4'
_chemical_formula_weight         2102.74
_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                85.150(1)
_cell_angle_beta                 89.605(1)
_cell_angle_gamma                75.421(1)
_cell_formula_units_Z            1
_cell_length_a                   9.2045(1)
_cell_length_b                   11.5410(2)
_cell_length_c                   23.4034(4)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.996
_cell_measurement_theta_min      3.792
_cell_volume                     2397.19(6)
_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      173(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0785
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            46089
_diffrn_reflns_theta_full        67.63
_diffrn_reflns_theta_max         67.63
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    3.814
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2010)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent plate'
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.007
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         8375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0503P)^2^+2.0443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                6554
_reflns_number_total             8375
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-400-228-238-2.cif
_cod_data_source_block           2a-[Cu(PPh3)2]2
_cod_database_code               1516951