Monomer‒polymer forms of solid, unsolvated, 5-coordinate halodimethyl(2-diphenylphosphinylethyl)stannanes, XMe2SnCH2CH2P(O)Ph2 (X = Cl, Br or I). Effects of different recrystallisation media
Harrison, William T. A.; Howie, R. Alan; Munro, Craig M.; Wardell, James L.; Journal of the Chemical Society, Dalton Transactions  (2001) 2593–; doi:10.1039/b103107b

data_7010738
_publ_section_title
;
 Monomer--polymer forms of solid, unsolvated, 5-coordinate
 halodimethyl(2-diphenylphosphinylethyl)stannanes, XMe2SnCH2CH2P(O)Ph2
 (X&#x00A0;=&#x00A0;Cl, Br or I). Effects of different
 recrystallisation media
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2593
_journal_paper_doi               10.1039/b103107b
_journal_year                    2001
_chemical_formula_moiety         'C16 H20 I O P Sn'
_chemical_formula_sum            'C16 H20 I O P Sn'
_chemical_formula_weight         504.88
_chemical_name_systematic
; 
Catena[iododimethyl(2-diphenylphosphinoethyl)stannane]
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7840(4)
_cell_length_b                   11.9471(5)
_cell_length_c                   14.2380(6)
_cell_measurement_reflns_used    7413
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      44.9
_cell_measurement_theta_min      2.5
_cell_volume                     1834.39(13)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11013
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.157
_exptl_absorpt_correction_T_max  0.8619
_exptl_absorpt_correction_T_min  0.6127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS: Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0185
_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^)+(0.0258P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0430
_refine_ls_wR_factor_ref         0.0436
_reflns_number_gt                3080
_reflns_number_total             3222
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b103107b.txt
_cod_data_source_block           iprt
_cod_database_code               7010738