P–N bond formation as a route to a highly electron rich bidentate phosphine ligand and its application in homogenous catalysis
Rodriguez i Zubiri, Mireia; Clarke, Matthew L.; Foster, Douglas F.; Cole-Hamilton, David J.; Slawin, Alexandra M. Z.; Woollins, J. Derek; Journal of the Chemical Society, Dalton Transactions  (2001) 969–; doi:10.1039/b101656n

data_7010649
_publ_section_title
;
 P--N bond formation as a route to a highly electron rich bidentate
 phosphine ligand and its application in homogenous catalysis
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              969
_journal_paper_doi               10.1039/b101656n
_journal_year                    2001
_chemical_formula_analytical     'C17 H38 N2 P2 Se2'
_chemical_formula_moiety         'C17 H38 N2 P2 Se2'
_chemical_formula_structural     'C17 H38 N2 P2 Se2'
_chemical_formula_sum            'C17 H38 N2 P2 Se2'
_chemical_formula_weight         490.35
_chemical_melting_point          ?
_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
_cell_angle_alpha                108.223(8)
_cell_angle_beta                 98.723(8)
_cell_angle_gamma                93.164(8)
_cell_formula_units_Z            2
_cell_length_a                   6.959(3)
_cell_length_b                   11.700(5)
_cell_length_c                   14.974(7)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      168
_cell_measurement_theta_min      12
_cell_volume                     1137.8(9)
_computing_cell_refinement       SMART/SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2600
_diffrn_reflns_av_sigmaI/netI    0.2393
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6629
_diffrn_reflns_theta_max         23.39
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    3.392
_exptl_absorpt_correction_T_max  0.42224
_exptl_absorpt_correction_T_min  0.31658
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    -
_exptl_crystal_description       plate
_exptl_crystal_F_000             504
_exptl_crystal_size_max          .14
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .01
_refine_diff_density_max         1.363
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.210
_refine_ls_extinction_coef       0.0000(27)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.841
_refine_ls_goodness_of_fit_obs   0.987
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_restrained_S_obs      0.987
_refine_ls_R_factor_all          0.2312
_refine_ls_R_factor_obs          0.1130
_refine_ls_shift/esd_max         -0.456
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.4165
_refine_ls_wR_factor_obs         0.2636
_reflns_number_observed          1295
_reflns_number_total             3281
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b101656n.txt
_cod_data_source_block           3Se
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/adriana/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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '-' was changed to '?' - the value is
undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.2276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010649