Lithium, Potassium, and Tin(II) Complexes of Novel 3-(Iminophosphorano)-1-phosphaallyl and 2-(Iminophosphorano)-1-phosphaallyl Ligands
Wang, Zhong-Xia; Li, Ye-Xin; Organometallics 21 (2002) 4641–; doi:10.1021/om020422c

data_4077015
_publ_section_title
;
 Lithium, Potassium, and Tin(II) Complexes of Novel
 3-(Iminophosphorano)-1-phosphaallyl and
 2-(Iminophosphorano)-1-phosphaallyl Ligands
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              4641
_journal_paper_doi               10.1021/om020422c
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C38 H52 N2 P4 Si2 Sn'
_chemical_formula_weight         835.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 96.580(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.605(4)
_cell_length_b                   11.840(2)
_cell_length_c                   18.611(4)
_cell_measurement_reflns_used    2442
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      21.720
_cell_measurement_theta_min      2.203
_cell_volume                     4291.6(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      299(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0892
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10545
_diffrn_reflns_theta_full        24.78
_diffrn_reflns_theta_max         24.78
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.7894
_exptl_absorpt_correction_T_min  0.7605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.31(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6513
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          2.578
_refine_ls_shift/su_mean         0.282
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                3814
_reflns_number_total             6513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020422c.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        4291.4(15)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4077015