Novel diphenylphosphine derivatives of 2,2′-bithiophene, 2,2′:5′,2″-terthiophene, 2-(2′-thienyl)pyridine and 2,6-di-2′-thienylpyridine. Crystal structures of 5,5′-bis(diphenylphosphino)-2,2′-bithiophene, diphenyl{5-[6′-(diphenylphosphino)-2′-pyridyl]-2-thienyl}phosphine and 2,6-bis[5′-(diphenylphosphino)-2′-thienyl]pyridine
; Journal of the Chemical Society, Perkin Transactions 1  (2001) 3352–; doi:10.1039/b107389n

data_7216888
_publ_contact_author             'Professor J. S. Field'
_publ_section_title
;
 Novel diphenylphosphine derivatives of 2,2&#x2032;-bithiophene,
 2,2&#x2032;:5&#x2032;,2&#x2033;-terthiophene,
 2-(2&#x2032;-thienyl)pyridine and 2,6-di-2&#x2032;-thienylpyridine.
 Crystal structures of
 5,5&#x2032;-bis(diphenylphosphino)-2,2&#x2032;-bithiophene,
 diphenyl{5-[6&#x2032;-(diphenylphosphino)-2&#x2032;-pyridyl]-2-thienyl}phosphine
 and 2,6-bis[5&#x2032;-(diphenylphosphino)-2&#x2032;-thienyl]pyridine
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              3352
_journal_paper_doi               10.1039/b107389n
_journal_year                    2001
_chemical_formula_moiety         '[{P(C6H5)2}2(C4H2S)2(C6H3N)2]'
_chemical_formula_sum            'C37 H27 N P2 S2'
_chemical_formula_weight         611.66
_chemical_melting_point          448.15
_chemical_name_systematic
;
2,6-bis[(5'-diphenylphosphino)-2'-thienyl]pyridine
;
_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                85.853(18)
_cell_angle_beta                 82.694(19)
_cell_angle_gamma                73.772(18)
_cell_formula_units_Z            2
_cell_length_a                   9.032(2)
_cell_length_b                   13.312(3)
_cell_length_c                   13.577(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      2
_cell_volume                     1553.5(6)
_computing_cell_refinement       'CELDIM, CAD4'
_computing_data_collection       'Nonius CAD4'
_computing_data_reduction        'XCAD (McArdle, 2000)'
_computing_molecular_graphics    'OSCAIL (McArdle 2000)'
_computing_publication_material  'ORTEP 3 (Farrugia, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius CAD4'
_diffrn_measurement_method       'omega-2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4946
_diffrn_reflns_theta_full        22.97
_diffrn_reflns_theta_max         22.97
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0%
_diffrn_standards_interval_time  '60 minutes'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   PSI-Scans
_exptl_absorpt_process_details
;
Walker, N. & Stuart, D. (1983) Acta. Cryst. A39, 158-166.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         4301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.4329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                3311
_reflns_number_total             4301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b107389n.txt
_cod_data_source_block           el04
_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 

The following automatic conversions were performed:

'_chemical_melting_point' value '175 C' was changed to '448.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1553.4(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7216888