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_4077014
_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            'C66 H112 Li2 N2 O4 P4 Si4'
_chemical_formula_weight         1247.70
_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                103.262(6)
_cell_angle_beta                 97.354(6)
_cell_angle_gamma                94.270(5)
_cell_formula_units_Z            4
_cell_length_a                   10.655(3)
_cell_length_b                   17.776(5)
_cell_length_c                   21.218(6)
_cell_measurement_reflns_used    846
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      15.516
_cell_measurement_theta_min      2.3o9
_cell_volume                     3856.9(19)
_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 0.932
_diffrn_measured_fraction_theta_max 0.932
_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  0.0895
_diffrn_reflns_av_sigmaI/netI    0.4420
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13982
_diffrn_reflns_theta_full        23.37
_diffrn_reflns_theta_max         23.37
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  0.9421
_exptl_absorpt_correction_T_min  0.9238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.644
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         10463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.644
_refine_ls_R_factor_all          0.2863
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                2231
_reflns_number_total             10463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020422c.cif
_cod_data_source_block           5
_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_cell_volume        3857(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077014