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_7216889
_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)(C5H3N)]'
_chemical_formula_sum            'C33 H25 N P2 S'
_chemical_formula_weight         529.54
_chemical_melting_point          432.15
_chemical_name_systematic
;
Diphenyl[5-(2'-{6'-diphenylphosphino}pyridyl)-2-thienyl]phosphine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.11(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.408(5)
_cell_length_b                   15.978(6)
_cell_length_c                   20.402(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      2
_cell_volume                     2689(2)
_computing_cell_refinement       'CELDIM, CAD4'
_computing_data_collection       'Nonius CAD4'
_computing_data_reduction        'XCAD (McArdle, 2000)'
_computing_molecular_graphics    'ORTEP 3  (Farrugia, 2000)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       1
_diffrn_reflns_number            3925
_diffrn_reflns_theta_full        22.98
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0%
_diffrn_standards_interval_time  '60 minutes'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details
;
Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0000P)^2^+4.3953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                2173
_reflns_number_total             3616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b107389n.txt
_cod_data_source_block           el08
_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 '159 C' was changed to '432.15' - it
was converted from degrees Celsius(C) to
Kelvins(K).

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2690(2)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7216889
_exptl-crystal_preparation
;
Crystals grown from petroleum ether/ether by slow evaporation
;