Steric and electronic control over the structural diversity of N-(n-pyridinyl) diphenylphosphinic amides (n = 2 and 4) as difunctional ligands in triphenyltin(iv) adducts
Gholivand, K.; Gholami, A.; Tizhoush, S. K.; Schenk, K. J.; Fadaei, F.; Bahrami, A.; RSC Adv. 4 (2014) 44509–; doi:10.1039/C4RA06212D

data_7218176
_publ_section_title
;
 Steric and electronic control over the structural diversity of
 N-(n-pyridinyl) diphenylphosphinic amides (n = 2 and 4) as difunctional
 ligands in triphenyltin(iv) adducts
;
_journal_issue                   84
_journal_name_full               'RSC Adv.'
_journal_page_first              44509
_journal_paper_doi               10.1039/C4RA06212D
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C35 H30 Cl N2 O P Sn, C17 H15 N2 O P'
_chemical_formula_sum            'C52 H45 Cl N4 O2 P2 Sn'
_chemical_formula_weight         974.00
_chemical_name_systematic
;
 [N-(4-pyridinyle)diphenylephosphinic amide-kappa-N chlorotriphenyltin(IV)].
 N-(4-pyridinyle)diphenylephosphinic amide
;
_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
_cell_angle_alpha                82.955(5)
_cell_angle_beta                 81.181(5)
_cell_angle_gamma                74.541(5)
_cell_formula_units_Z            2
_cell_length_a                   9.9181(6)
_cell_length_b                   14.7686(9)
_cell_length_c                   16.9564(10)
_cell_measurement_reflns_used    64411
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      29.70
_cell_measurement_theta_min      1.44
_cell_volume                     2356.8(3)
_computing_cell_refinement       'X_Area, 1.36 (Stoe, 2006)'
_computing_data_collection       'X_Area, 1.36 (Stoe, 2006)'
_computing_data_reduction        'X_Area, 1.36 (Stoe, 2006)'
_computing_molecular_graphics    'Bruker SHELXTL, (Bruker, 1996)'
_computing_publication_material  'Bruker SHELXTL, PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF, Release 2008.3 (2008)'
_diffrn_ambient_temperature      292
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      ' 397 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46955
_diffrn_reflns_theta_full        29.31
_diffrn_reflns_theta_max         29.31
_diffrn_reflns_theta_min         1.80
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           43
_diffrn_source_power             2.365
_diffrn_source_voltage           55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.71
_exptl_absorpt_correction_T_max  0.9079
_exptl_absorpt_correction_T_min  0.7211
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Stoe XRed32 1.31, Stoe (2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.347
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.818
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0199(11)
_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_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         12706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0832P)^2^+1.0906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1557
_reflns_number_gt                9504
_reflns_number_total             12706
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4ra06212d2.cif
_cod_data_source_block           MrSOSO
_cod_original_cell_volume        2356.8(2)
_cod_database_code               7218176