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_4076254
_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            'C40 H85 O7 P3 Sn2'
_chemical_formula_weight         1008.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.758(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.512(3)
_cell_length_b                   17.259(3)
_cell_length_c                   18.228(4)
_cell_measurement_temperature    150(2)
_cell_volume                     5066.4(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23081
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.112
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         8938
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0518P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                5609
_reflns_number_total             8938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om034262wsi20031027_115228.cif
_cod_data_source_block           vc25m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5066.3(17)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4076254