Very large changes in bond length and bond angle in a heavy group 14 element alkyne analogue by modification of a remote ligand substituent.
Fischer, Roland C; Pu, Lihung; Fettinger, James C; Brynda, Marcin A; Power, Philip P; Journal of the American Chemical Society 128 (2006) 11366–11367; doi:10.1021/ja0637090

data_4101581
_publ_section_title
;
 Very large changes in bond length and bond angle in a heavy group 14
 element alkyne analogue by modification of a remote ligand
 substituent.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11366
_journal_page_last               11367
_journal_paper_doi               10.1021/ja0637090
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         '2(C33 H45 Si Sn), C4 H10 O'
_chemical_formula_sum            'C70 H100 O Si2 Sn2'
_chemical_formula_weight         1251.06
_chemical_melting_point          184.0(10)
_chemical_name_systematic        {[4-Me3Si-2,6-(2,6-iPr2-C6H3)2-C6H2]Sn}2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 114.407(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.605(3)
_cell_length_b                   24.573(5)
_cell_length_c                   12.733(3)
_cell_measurement_reflns_used    4275
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.46
_cell_measurement_theta_min      2.17
_cell_volume                     3306.5(12)
_computing_cell_refinement       'SAINT (7.23A) (Bruker, 2005)'
_computing_data_collection       'SMART (Version 5.054) (Bruker, 2002)'
_computing_data_reduction        'SAINT (7.23A) (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART1000'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1290
_diffrn_reflns_av_sigmaI/netI    0.1230
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23348
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.93
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.9365
_exptl_absorpt_correction_T_min  0.8448
_exptl_absorpt_correction_type   'Empirical, SADABS (multi-scan)'
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1312
_exptl_crystal_recrystallization_method Diethylether
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.077
_refine_diff_density_min         -1.476
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5975
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0365P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                3272
_reflns_number_total             5975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0637090si20060526_072032.cif
_cod_data_source_block           1395ffmi
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '183-185' was changed to '184.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4101581