First Isocyanoazulene and Its Homoleptic Complexes
Randall E. Robinson; Thomas C. Holovics; Stephan F. Deplazes; Gerald H. Lushington; Douglas R. Powell; Mikhail V. Barybin; Journal of the American Chemical Society 125 (2003) 4432–4433; doi:10.1021/ja034706f

data_4113659
_publ_contact_author
; 
   Prof. Mikhail V. Barybin 
   Department of Chemistry 
   University of Kansas 
   Rm 2010 Malott Hall
   1251 Wescoe Hall Dr. 
   Lawrence, KS  66045-7582  USA 
;
_publ_contact_author_email       mbarybin
_publ_contact_author_fax         1(785)8645396
_publ_contact_author_phone       1(785)8644090
_publ_section_title
;
 First Isocyanoazulene and Its Homoleptic Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4432
_journal_page_last               4433
_journal_paper_doi               10.1021/ja034706f
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C66 H42 B Cr F4 N6'
_chemical_formula_sum            'C66 H42 B Cr F4 N6'
_chemical_formula_weight         1057.87
_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                 106.973(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.934(7)
_cell_length_b                   13.572(5)
_cell_length_c                   21.073(7)
_cell_measurement_reflns_used    1628
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.86
_cell_measurement_theta_min      2.25
_cell_volume                     5453(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scan frames'
_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  0.1797
_diffrn_reflns_av_sigmaI/netI    0.1352
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9772
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        -0.12
_diffrn_standards_number         64
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.9813
_exptl_absorpt_correction_T_min  0.9064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 2000'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         2853
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0920P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1733
_reflns_number_gt                1843
_reflns_number_total             2853
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034706fsi20030216_014050.cif
_cod_data_source_block           compound_2_
_cod_database_code               4113659