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_4063912
_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         'C28 H40 O8 P2'
_chemical_formula_sum            'C28 H40 O8 P2'
_chemical_formula_weight         566.54
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.1240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.3095(6)
_cell_length_b                   11.2676(2)
_cell_length_c                   8.6835(2)
_cell_measurement_reflns_used    15940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.78
_cell_volume                     2838.93(10)
_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      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.366
_diffrn_detector_type            'Bruker-AXS SMART APEX'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15508
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.94
_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    0.201
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.173
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0442P)^2^+2.7243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                3059
_reflns_number_total             3275
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101023e_si_001.cif
_cod_data_source_block           migl7_c2c
_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_sg_symbol_H-M      'C 2/c'
_cod_database_code               4063912