Synthesis and Study of the First N-Aryl Acyclic Diaminocarbene and Its Transition-Metal Complexes
Rosen, Evelyn L.; Sanderson, Matthew D.; Saravanakumar, Shanmuganathan; Bielawski, Christopher W.; Organometallics 26 (2007) 5774–; doi:10.1021/om7007925

data_4072440
_publ_section_title
;
 Synthesis and Study of the First N-Aryl Acyclic Diaminocarbene and Its
 Transition-Metal Complexes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5774
_journal_paper_doi               10.1021/om7007925
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C33 H37 N4 O4 1+, Br 1-, 1.5 C4 H8 O'
_chemical_formula_sum            'C39 H47 Br N4 O5.5'
_chemical_formula_weight         739.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 95.8360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.8293(5)
_cell_length_b                   8.9223(1)
_cell_length_c                   25.9432(6)
_cell_measurement_temperature    153(2)
_cell_volume                     7559.7(2)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0641
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21397
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'de Meulenaar, J., Tompa, H. (1965) Acta Cryst. A19, 1014-1018'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8419
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+5.9840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1134
_reflns_number_gt                6078
_reflns_number_total             8419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cif.cif
_cod_data_source_block           elr1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Analytical'
changed to 'analytical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C39 H47 Br N4 O5.50'
_cod_database_code               4072440