Multifunctional Dithiocarbamates: Synthesis and Ring-Closing Metathesis of Diallyldithiocarbamate Complexes
Naeem, Saira; White, Andrew J. P.; Hogarth, Graeme; Wilton-Ely, James D. E. T.; Organometallics 29 (2010) 2547–; doi:10.1021/om1002123

data_4065959
_publ_section_title
;
 Multifunctional Dithiocarbamates: Synthesis and Ring-Closing Metathesis
 of Diallyldithiocarbamate Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2547
_journal_paper_doi               10.1021/om1002123
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C32 H32 N Ni P2 S2, (F6 P), 1.75(C H Cl3)'
_chemical_formula_sum            'C33.75 H33.75 Cl5.25 F6 N Ni P3 S2'
_chemical_formula_weight         969.22
_chemical_name_systematic
; 
 ? 
;
_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                92.0086(14)
_cell_angle_beta                 102.8560(19)
_cell_angle_gamma                98.9786(18)
_cell_formula_units_Z            4
_cell_length_a                   13.7545(4)
_cell_length_b                   15.2829(3)
_cell_length_c                   20.3044(4)
_cell_measurement_reflns_used    18718
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.8170
_cell_measurement_theta_min      2.9597
_cell_volume                     4099.38(17)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            39906
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         31.89
_diffrn_reflns_theta_min         2.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) 
(compiled Sep 15 2009,11:49:04) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1966
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         24642
_refine_ls_number_restraints     1752
_refine_ls_restrained_S_all      1.344
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                16353
_reflns_number_total             24642
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1002123_si_002.cif
_cod_data_source_block           15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065959