Fine Tuning of the Substituents on the N-Geminal Phosphorus/Silicon-Based Lewis Pairs for the Synthesis ofZ-Type Silyliminophosphoranylalkenes
Li, Jiancheng; Li, Yan; Purushothaman, Indu; De, Susmita; Li, Bin; Zhu, Hongping; Parameswaran, Pattiyil; Ye, Qingsong; Liu, Weiping; Organometallics 34 (2015) 4209–; doi:10.1021/om501288t

data_4085727
_publ_section_title
;
 Fine Tuning of the Substituents on the N-Geminal Phosphorus/Silicon-Based
 Lewis Pairs for the Synthesis ofZ-Type Silyliminophosphoranylalkenes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4209
_journal_paper_doi               10.1021/om501288t
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C31.5 H34 Cl7.5 N O4 P Si'
_chemical_formula_weight         815.53
_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                104.084(5)
_cell_angle_beta                 101.275(5)
_cell_angle_gamma                99.312(5)
_cell_formula_units_Z            2
_cell_length_a                   9.8723(6)
_cell_length_b                   12.2232(7)
_cell_length_c                   16.7314(9)
_cell_measurement_reflns_used    4222
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.8300
_cell_measurement_theta_min      3.3960
_cell_volume                     1873.4(2)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_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 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w 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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14342
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.8228
_exptl_absorpt_correction_T_min  0.8228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             837
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.291
_refine_diff_density_min         -1.701
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7352
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+4.8436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.1873
_reflns_number_gt                5834
_reflns_number_total             7352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501288t_si_003.cif
_cod_data_source_block           compound_5b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4085726--4085732.cif.
;
_cod_original_cell_volume        1873.40(19)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C31.50 H34 Cl7.50 N O4 P Si'
_cod_database_code               4085727