Cage Phosphinites: Ligands for Efficient Nickel-Catalyzed Hydrocyanation of 3-Pentenenitrile
Mikhel, Igor S.; Garland, Michael; Hopewell, Jonathan; Mastroianni, Sergio; McMullin, Claire L.; Orpen, A. Guy; Pringle, Paul G.; Organometallics 30 (2011) 974–; doi:10.1021/om101023e

data_4063917
_publ_section_title
;
 Cage Phosphinites: Ligands for Efficient Nickel-Catalyzed Hydrocyanation
 of 3-Pentenenitrile
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              974
_journal_paper_doi               10.1021/om101023e
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C64 H92 Ni2 O16 P4, 2(C7 H8), C7 H7'
_chemical_formula_sum            'C85 H115 Ni2 O16 P4'
_chemical_formula_weight         1634.03
_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                93.92(2)
_cell_angle_beta                 103.44(3)
_cell_angle_gamma                114.257(17)
_cell_formula_units_Z            2
_cell_length_a                   11.489(4)
_cell_length_b                   11.686(3)
_cell_length_c                   17.003(8)
_cell_measurement_reflns_used    5231
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.33
_cell_volume                     1989.4(14)
_computing_cell_refinement       'Apex II (Bruker-AXS, 2007)'
_computing_data_collection       'Apex II (Bruker-AXS, 2007)'
_computing_data_reduction
; 
 SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.366
_diffrn_detector_type            'Bruker-AXS SMART APEX'
_diffrn_measured_fraction_theta_full 0.578
_diffrn_measured_fraction_theta_max 0.578
_diffrn_measurement_details      'frames, 0.3\% width'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker-AXS Kappa'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_measurement_specimen_support
; 
glass fibre 
;
_diffrn_radiation_collimation    '0.5 mm double pinhole'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71074
_diffrn_reflns_av_R_equivalents  0.0947
_diffrn_reflns_av_sigmaI/netI    0.2915
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8870
_diffrn_reflns_theta_full        27.40
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         1.95
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           40
_diffrn_source_power             2
_diffrn_source_size              '0.4 x 8 mm fine focus'
_diffrn_source_target            Mo
_diffrn_source_type              'Bruker-AXS KFF Mo 2K 90\% Ceramic'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2 (Sheldrick, G.M., 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             869
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         5230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.2156
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.2141
_reflns_number_gt                2044
_reflns_number_total             5230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101023e_si_001.cif
_cod_data_source_block           migl7_ni_p_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' 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        1989.4(12)
_cod_database_code               4063917