Reactions ofn-Bu2SnO and (n-Bu3Sn)2O with 1,1,2,3,3-Pentamethyltrimethylene Phosphinic Acid: Synthesis and X-ray Crystal Structures of a Novel Spirocyclic Coordination Polymer and a 16-Membered Inorganic Macrocycle
Chandrasekhar, Vadapalli; Baskar, Viswanathan; Steiner, Alexander; Zacchini, Stefano; Organometallics 23 (2004) 1390–; doi:10.1021/om034262w

data_4076255
_publ_section_title
;
 Reactions ofn-Bu2SnO and (n-Bu3Sn)2O with
 1,1,2,3,3-Pentamethyltrimethylene Phosphinic Acid:&#x00A0; Synthesis and
 X-ray Crystal Structures of a Novel Spirocyclic Coordination Polymer and
 a 16-Membered Inorganic Macrocycle
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1390
_journal_paper_doi               10.1021/om034262w
_journal_volume                  23
_journal_year                    2004
_chemical_formula_sum            'C80 H172 O8 P4 Sn4'
_chemical_formula_weight         1860.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.2108(8)
_cell_length_b                   19.2108(8)
_cell_length_c                   13.0532(7)
_cell_measurement_temperature    150(2)
_cell_volume                     4817.3(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS Smart Apex'
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            25001
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         4267
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0566P)^2^+8.1733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                3166
_reflns_number_total             4267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om034262wsi20031027_115228.cif
_cod_data_source_block           vc24m
_cod_original_sg_symbol_H-M      P4(2)/n
_cod_database_code               4076255