Coordination Chemistry of a Bicyclic 3-Aza-7-phosphabicyclo[3.3.1]nonan-9-one Ligand
Zayya, Almas I.; Spencer, John L.; Organometallics 31 (2012) 2841–; doi:10.1021/om201131w

data_4077964
_publ_section_title
;
 Coordination Chemistry of a Bicyclic
 3-Aza-7-phosphabicyclo[3.3.1]nonan-9-one Ligand
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2841
_journal_paper_doi               10.1021/om201131w
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C39 H55.86 N3 O5.43 P Pt, C9 H5 F6 O4 S2'
_chemical_formula_sum            'C48 H60 F6 N3 O9 P Pt S2'
_chemical_formula_weight         1227.17
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2011-11-08
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_cell_angle_alpha                91.528(2)
_cell_angle_beta                 97.270(2)
_cell_angle_gamma                114.749(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3130(4)
_cell_length_b                   14.9607(5)
_cell_length_c                   16.1929(5)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    119(2)
_cell_measurement_theta_max      30.89
_cell_measurement_theta_min      2.28
_cell_volume                     2894.02(17)
_computing_data_reduction        'SAINT v7.53A (Bruker, 2008)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      119(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            88285
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         35.21
_diffrn_reflns_theta_min         1.27
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.593
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.5850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
"SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0811 before and 0.0508 after correction.
The Ratio of minimum to maximum transmission is 0.7832.
The \l/2 correction factor is 0.00.
{Info from C:\Users\Brad\Desktop\Almas xtal\BGA soln p-1\pnc_ac.abs}
;
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.38
_refine_diff_density_max         1.647
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         21639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0483P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                18162
_reflns_number_total             21639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201131w_si_002.cif
_cod_data_source_block           pnc_ac
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        2894.01(16)
_cod_database_code               4077964