New Approach to the Synthesis of Azinylcymantrenes
Utepova, Irina A.; Musikhina, Alexandra A.; Chupakhin, Oleg N.; Slepukhin, Pavel A.; Organometallics 30 (2011) 3047–; doi:10.1021/om200159f

data_4064523
_publ_section_title
;
 New Approach to the Synthesis of Azinylcymantrenes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3047
_journal_paper_doi               10.1021/om200159f
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C16 H9 Mn N2 O3'
_chemical_formula_sum            'C16 H9 Mn N2 O3'
_chemical_formula_weight         332.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 114.609(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1631(14)
_cell_length_b                   12.7084(16)
_cell_length_c                   11.9261(19)
_cell_measurement_reflns_used    2315
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.74
_cell_volume                     1400.4(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
;
_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      295(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
  1 omega   41.00  111.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       32.0000 -170.0000   30.0000    0.0000    0.0000 70

  2 omega  -39.00   51.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       32.0000  -80.0000   30.0000    0.0000    0.0000 90

  3 omega  -29.00   71.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       32.0000  -90.0000   50.0000    0.0000    0.0000 100

  4 omega  -29.00   -3.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       32.0000  -10.0000   20.0000    0.0000    0.0000 26

;
_diffrn_measurement_device_type  'Xcalibur 3 CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_orient_matrix_UB_11      -0.0194109487
_diffrn_orient_matrix_UB_12      0.0537951862
_diffrn_orient_matrix_UB_13      -0.0013158857
_diffrn_orient_matrix_UB_21      -0.0224887038
_diffrn_orient_matrix_UB_22      -0.0094838004
_diffrn_orient_matrix_UB_23      0.0473823507
_diffrn_orient_matrix_UB_31      0.0716105629
_diffrn_orient_matrix_UB_32      0.0116036046
_diffrn_orient_matrix_UB_33      0.0451767983
_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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4351
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.2144
_exptl_crystal_size_mid          0.1307
_exptl_crystal_size_min          0.0701
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                2315
_reflns_number_total             3348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200159f_si_002.cif
_cod_data_source_block           dc4h
_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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1400.4(3)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4064523