Sn(II)–Carbon Bond Reactivity: Radical Generation and Consumption via Reactions of a Stannylene with Alkynes
Zou, Wenxing; Mears, Kristian; Fettinger, James C.; Power, Philip P.; Chemical Communications  (2023) –; doi:10.1039/D3CC04014C

data_7132182
_publ_section_title
;
 Sn(II)--Carbon Bond Reactivity: Radical Generation and Consumption via
 Reactions of a Stannylene with Alkynes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04014C
_journal_year                    2023
_chemical_formula_moiety         'C72 H90 O Sn'
_chemical_formula_sum            'C72 H90 O Sn'
_chemical_formula_weight         1090.12
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-09-27 deposited with the CCDC.	2023-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                88.9389(8)
_cell_angle_beta                 81.5494(8)
_cell_angle_gamma                89.9199(8)
_cell_formula_units_Z            4
_cell_length_a                   17.8418(9)
_cell_length_b                   17.8598(9)
_cell_length_c                   19.2380(10)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.28
_cell_volume                     6062.6(5)
_computing_cell_refinement       'SAINT (8.38a) (Bruker, 2017)'
_computing_data_collection       'Apex3 (2019.1) (Bruker, 2019)'
_computing_data_reduction        'SAINT (8.38a) (Bruker, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43731
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         1.837
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_T_max  0.9240
_exptl_absorpt_correction_T_min  0.8027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Sheldrick, 2016)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       Block
_exptl_crystal_F_000             2320
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.188
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1434
_refine_ls_number_reflns         21950
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0067P)^2^+15.6202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15968
_reflns_number_total             21950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04014c4.cif
_cod_data_source_block           WZ13FMI
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7132182
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.878
_shelx_estimated_absorpt_t_max   0.918
_shelx_res_checksum              84282
_shelx_hkl_checksum              9121