Synthesis of chiral organotin reagents: synthesis of enantiomerically enriched bicyclo[2.2.1]hept-2-yl tin hydrides from camphor. X-Ray crystal structures of (dimethyl)[(1R,2S,4R)-1,7,7-trimethylbicyclo[2.2.1]hept-2-yl]tin chloride and methyl(phenyl)bis[(1R,2S,4R)-1,7,7-trimethylbicyclo[2.2.1]hept-2-yl]stannane
Helliwell, Madeleine; Thomas, Eric J.; Townsend, Linda A.; Journal of the Chemical Society, Perkin Transactions 1  (2002) 1286–; doi:10.1039/b200317c

data_7204350
_publ_section_title
;
 Synthesis of chiral organotin reagents: synthesis of enantiomerically
 enriched bicyclo[2.2.1]hept-2-yl tin hydrides from camphor. X-Ray
 crystal structures of
 (dimethyl)[(1R,2S,4R)-1,7,7-trimethylbicyclo[2.2.1]hept-2-yl]tin
 chloride and
 methyl(phenyl)bis[(1R,2S,4R)-1,7,7-trimethylbicyclo[2.2.1]hept-2-yl]stannane
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1286
_journal_paper_doi               10.1039/b200317c
_journal_year                    2002
_chemical_formula_moiety         'C27 H42 Sn '
_chemical_formula_sum            'C27 H42 Sn'
_chemical_formula_weight         485.32
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             19101-12-11
_audit_creation_method           'by teXsan v1.7'
_audit_update_record             ?
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.072(2)
_cell_length_b                   25.978(3)
_cell_length_c                   9.617(2)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      39.6
_cell_measurement_theta_min      31.8
_cell_volume                     2516.3(8)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.05250
_diffrn_orient_matrix_UB_12      0.01992
_diffrn_orient_matrix_UB_13      0.06994
_diffrn_orient_matrix_UB_21      -0.01805
_diffrn_orient_matrix_UB_22      -0.03246
_diffrn_orient_matrix_UB_23      0.05260
_diffrn_orient_matrix_UB_31      0.08231
_diffrn_orient_matrix_UB_32      0.00559
_diffrn_orient_matrix_UB_33      0.05615
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.00000
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2769
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         79.19
_diffrn_reflns_theta_min         3.40
_diffrn_standards_decay_%        -3.49
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.301
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_meas      ?
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1016.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.64
_refine_ls_abs_structure_Flack   0.019(5)
_refine_ls_extinction_coef       0.00000016(4)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   2.086
_refine_ls_goodness_of_fit_obs   2.149
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2438
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_obs          0.0358
_refine_ls_shift/esd_max         0.0000
_refine_ls_shift/esd_mean        0.2580
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0292
_refine_ls_wR_factor_obs         0.0282
_reflns_number_observed          2438
_reflns_number_total             2769
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            b200317c.txt
_cod_data_source_block           s658
_cod_depositor_comments
;
 Correcting the data name order in the GEOM_TORSION loop.

 Antanas Vaitkus,
 2018-08-08

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00000|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2516.2(6)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C27 H42 Sn '
_cod_database_code               7204350