Synthesis and Reactivity of Intramolecularly NHC-Stabilized Germylenes and Stannylenes
Paul, Daniel; Heins, Frederik; Krupski, Sergei; Hepp, Alexander; Daniliuc, Constantin G.; Klahr, Kevin; Neugebauer, Johannes; Glorius, Frank; Hahn, F. Ekkehardt; Organometallics  (2017) –; doi:10.1021/acs.organomet.6b00925

data_4087065
_publ_section_title
;
 Synthesis and Reactivity of Intramolecularly NHC-Stabilized Germylenes
 and Stannylenes
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.6b00925
_journal_year                    2017
_chemical_formula_sum            'C25 H32 Cl N3 O0.5 Sn'
_chemical_formula_weight         536.67
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.8040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.2740(4)
_cell_length_b                   12.2320(6)
_cell_length_c                   49.393(2)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.527
_cell_measurement_theta_min      2.3475
_cell_volume                     4981.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            143770
_diffrn_reflns_theta_full        30.57
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    1.152
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.713
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         15264
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0454P)^2^+5.1263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                11310
_reflns_number_total             15264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00925_si_002.cif
_cod_data_source_block           '[3b]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

2026-05-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C50 H64 Cl2 N6 O Sn2'
_cod_original_formula_weight         1073.35
_cod_original_formula_units_Z            4
_cod_database_code               4087065