Access to new Janus head ligands: linking sulfur diimides and phosphanes for hemilabile tripodal scorpionates.
Meinholz, Margret M.; Pandey, Sushil K.; Deuerlein, Stephan M.; Stalke, Dietmar; Dalton transactions (Cambridge, England : 2003) 40 (2011) 1662–1671; doi:10.1039/c0dt00665c

data_7014374
_publ_section_title
;
 Access to new Janus head ligands: linking sulfur diimides and
 phosphanes for hemilabile tripodal scorpionates.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1662
_journal_page_last               1671
_journal_paper_doi               10.1039/c0dt00665c
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C22 H52 Li2 N4 P2 S2'
_chemical_formula_weight         512.62
_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                98.7720(10)
_cell_angle_beta                 92.0040(10)
_cell_angle_gamma                114.7780(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4916(4)
_cell_length_b                   9.6726(4)
_cell_length_c                   18.7808(8)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.74
_cell_measurement_theta_min      2.208
_cell_volume                     1537.77(11)
_computing_cell_refinement       'SAINT V7.46A'
_computing_data_collection       'APEX2 v2.2-0'
_computing_data_reduction        'SAINT V7.46A'
_computing_molecular_graphics    'XSHELL v4.01'
_computing_structure_refinement  'SHELXL in SHELXTL v2008/4 (Sheldrick 2008)'
_computing_structure_solution    'SHELXS in SHELXTL v2008/4 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker TXS-Mo rotating anode'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Helios mirror optics'
_diffrn_radiation_source         'Bruker TXS-Mo rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27095
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  0.9893
_exptl_absorpt_correction_T_min  0.7806
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         7923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0318P)^2^+0.4680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0693
_reflns_number_gt                6893
_reflns_number_total             7923
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT00665C.TXT
_cod_data_source_block           p-1a
_cod_original_cell_volume        1537.76(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7014374