Carbonylation of the simplest persistent diaminocarbene
Tim Schulz; Christian Farber; Michael Leibold; Clemens Bruhn; Wolfgang Baumann; Detlef Selent; Timo Porsch; Max C. Holthausen; Ulrich Siemeling; Chem.Commun. 49 (2013) 6834–; doi:10.1039/c3cc42888e

data_7109547
_publ_section_title
;
 Carbonylation of the simplest persistent diaminocarbene
;
_journal_name_full               Chem.Commun.
_journal_page_first              6834
_journal_paper_doi               10.1039/c3cc42888e
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C33 H72 Cl3 Li3 N12 O3'
_chemical_formula_sum            'C33 H72 Cl3 Li3 N12 O3'
_chemical_formula_weight         812.20
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 125.025(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.776(3)
_cell_length_b                   13.2356(13)
_cell_length_c                   18.2673(18)
_cell_measurement_reflns_used    8663
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.53
_cell_measurement_theta_min      1.86
_cell_volume                     4707.5(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      ' 162 frames, detector distance = 135 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13441
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           30
_diffrn_source_power             1.50
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_T_max  0.9841
_exptl_absorpt_correction_T_min  0.9534
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-red ver. 1.31 (Stoe & Cie. 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.147
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.030
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                2676
_reflns_number_total             4142
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc42888e.txt
_cod_data_source_block           i1103
_cod_original_cell_volume        4707.4(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7109547