Synthesis and reactivity of diphosphine metal complexes bearing peripheral ketenimine functionalities
Ruiz, Javier; Gonzalo, Marta P.; Vivanco, Marilín; Quesada, Roberto; Mosquera, Marta E. G.; Dalton Transactions  (2009) 9280–; doi:10.1039/b903375k

data_7002628
_publ_section_title
;
 Synthesis and reactivity of diphosphine metal complexes bearing
 peripheral ketenimine functionalities
;
_journal_issue                   42
_journal_name_full               'Dalton Transactions'
_journal_page_first              9280
_journal_paper_doi               10.1039/b903375k
_journal_year                    2009
_chemical_formula_moiety         ' C96 H75 Ag3 I2 N3 P6, Cl O4, C6 H14'
_chemical_formula_sum            'C102 H89 Ag3 Cl I2 N3 O4 P6'
_chemical_formula_weight         2219.44
_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                110.960(2)
_cell_angle_beta                 104.228(2)
_cell_angle_gamma                92.629(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8216(5)
_cell_length_b                   19.2320(7)
_cell_length_c                   20.9922(8)
_cell_measurement_reflns_used    1658
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      70.076
_cell_measurement_theta_min      1.767
_cell_volume                     4634.1(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000) '
_computing_data_reduction
'HKL Denzo & Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2000)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  kappaCCD
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27111
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.933
_exptl_absorpt_correction_T_max  0.7092
_exptl_absorpt_correction_T_min  0.3798
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_platon_squeeze_details
; A molecule of hexane crystallize with every molecule of this compound but
presented severe disorder and it was not possible to get a chemical sensible
model for it, so Squeeze procedure was used to remove their contribution
to the structure factors.
;
_refine_diff_density_max         1.282
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1051
_refine_ls_number_reflns         15745
_refine_ls_number_restraints     953
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0969P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                12264
_reflns_number_total             15745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903375k.txt
_cod_data_source_block           5b
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7002628