Synthesis of a Tetranuclear Organooxotin Cage by Debenzylation Reactions: X-ray Crystal Structure of [(PhCH2)2Sn2O(O2P(OH)-t-Bu)4]2
Chandrasekhar, Vadapalli; Baskar, Viswanathan; Steiner, Alexander; Zacchini, Stefano; Organometallics 21 (2002) 4528–; doi:10.1021/om020531r

data_4077066
_publ_section_title
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 Synthesis of a Tetranuclear Organooxotin Cage by Debenzylation
 Reactions:&#x00A0; X-ray Crystal Structure of
 [(PhCH2)2Sn2O(O2P(OH)-t-Bu)4]2
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_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4528
_journal_paper_doi               10.1021/om020531r
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C44.67 H72 O17.33 P5.33 Sn2.67'
_chemical_formula_weight         1368.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_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            6
_cell_length_a                   21.774(4)
_cell_length_b                   24.507(5)
_cell_length_c                   16.699(3)
_cell_measurement_temperature    150(2)
_cell_volume                     8911(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker AXS Smart Apex'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            30976
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block_like
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         5513
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+4.0214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                4916
_reflns_number_total             5513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020531r.cif
_cod_data_source_block           vc9new
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthorombic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      Pnna
_cod_database_code               4077066