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_7014379
_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            'C32 H56 Li2 N4 P2 S2'
_chemical_formula_weight         636.75
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.279(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5006(14)
_cell_length_b                   20.753(3)
_cell_length_c                   8.5699(11)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.7055
_cell_measurement_theta_min      2.1875
_cell_volume                     1852.5(4)
_computing_cell_refinement       'SAINT V7.46A'
_computing_data_collection       'Apex v2.2-0'
_computing_data_reduction        'SAINT V7.46A'
_computing_molecular_graphics    'XSHELL v4.01'
_computing_publication_material  'XSHELL v4.01'
_computing_structure_refinement  'SHELXL in SHELXTL 2008/2 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS in SHELXTL 2008/2 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC quazar mirror optics'
_diffrn_radiation_source         'INCOATEC Mo micro source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            39157
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.9703
_exptl_absorpt_correction_T_min  0.9358
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+1.0430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                3561
_reflns_number_total             3784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT00665C.TXT
_cod_data_source_block           p21c
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7014379