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_7014380
_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_moiety         'C27.50 H52 Li N4 P S Si2'
_chemical_formula_sum            'C27.5 H52 Li N4 P S Si2'
_chemical_formula_weight         564.88
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.895(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.944(5)
_cell_length_b                   9.5352(13)
_cell_length_c                   21.921(3)
_cell_measurement_reflns_used    8986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.577
_cell_measurement_theta_min      2.222
_cell_volume                     6942.7(17)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX v2009.11-0'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XSHELL v4.01'
_computing_structure_refinement  'SHELXL in SHELXTL v2008/4'
_computing_structure_solution    'SHELXS in SHELXTL v2008/4'
_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  0.0632
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            48696
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.9422
_exptl_absorpt_correction_T_min  0.8424
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS 2008-2'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         6847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0288P)^2^+8.9902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                5585
_reflns_number_total             6847
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT00665C.TXT
_cod_data_source_block           c2c2
_cod_original_cell_volume        6942.4(17)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C27.50 H52 Li N4 P S Si2'
_cod_database_code               7014380