Dibenzo[f,h]quinoline Cr(CO)3Complexes: Synthesis by Chromium-Templated Benzannulation, Cyclomanganation, and Haptotropic Chromium Migration
Dubarle Offner, Julien; Schnakenburg, Gregor; Rose-Munch, Françoise; Rose, Eric; Dötz, Karl Heinz; Organometallics 29 (2010) 3308–; doi:10.1021/om100258c

data_4066042
_publ_section_title
;
 Dibenzo[f,h]quinoline Cr(CO)3Complexes: Synthesis by Chromium-Templated
 Benzannulation, Cyclomanganation, and Haptotropic Chromium Migration
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3308
_journal_paper_doi               10.1021/om100258c
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C31 H35 Cr N O5 Si, C H2 Cl2'
_chemical_formula_sum            'C32 H37 Cl2 Cr N O5 Si'
_chemical_formula_weight         666.62
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                78.377(2)
_cell_angle_beta                 80.366(2)
_cell_angle_gamma                63.336(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5995(4)
_cell_length_b                   10.4632(4)
_cell_length_c                   18.2902(8)
_cell_measurement_reflns_used    39536
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      34.975
_cell_measurement_theta_min      0.998
_cell_volume                     1601.84(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20658
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.85549
_exptl_absorpt_correction_T_min  0.70513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         9304
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0766P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1442
_reflns_number_gt                6528
_reflns_number_total             9304
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om100258c_si_001.cif
_cod_data_source_block           GDOE019
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' 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        1601.84(11)
_cod_database_code               4066042