CNR and CO Insertion Reactions of 2,6-Xylyl Isocyanide withp-Chlorobenzylpentacarbonylmanganese
Becker, Thomas M.; Alexander, John J.; Krause Bauer, Jeanette A.; Nauss, Jeffrey L.; Wireko, Fred C.; Organometallics 18 (1999) 5594–; doi:10.1021/om9903644

data_4077806
_publ_section_title
;
 CNR and CO Insertion Reactions of 2,6-Xylyl Isocyanide
 withp-Chlorobenzylpentacarbonylmanganese
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5594
_journal_paper_doi               10.1021/om9903644
_journal_volume                  18
_journal_year                    1999
_chemical_compound_source        'see text'
_chemical_formula_sum            'C37 H33 Cl Mn N3 O3'
_chemical_formula_weight         658.05
_chemical_name_systematic
; 
1,1,1-tricarbonyl-1-[2,6-(dimethylphenyl)isocyanide]-2-[2,6-(dimethylphenyl)
imino]-3-(p-chlorobenzyl)-4-[2,6-(dimethylphenyl)]-4-azamangancylobut-3-ene 
 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXTL v5.03'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.239(6)
_cell_length_b                   15.971(5)
_cell_length_c                   23.062(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      5
_cell_volume                     6718(4)
_computing_cell_refinement       TEXSAN
_computing_data_collection       'TEXSAN (Molec. Struct. Corp.'
_computing_data_reduction        TEXSAN
_computing_molecular_graphics    'SHELXTL v5.03'
_computing_publication_material  'SHELXTL v5.03'
_computing_structure_refinement  'SHELXTL v5.03'
_computing_structure_solution    'SHELXTL v5.03 (Siemens, 1994)'
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \q--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2197
_diffrn_reflns_av_sigmaI/netI    0.2644
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5183
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        4.4
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.242
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7645
_exptl_absorpt_correction_type   'psi scans'
_exptl_absorpt_process_details   'North, Acta Cryst. (1968), A24, 351'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00042(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         4976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.2871
_refine_ls_R_factor_gt           0.0882
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0903P)^2^+23.8669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.2975
_reflns_number_gt                1797
_reflns_number_total             4988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9903644.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        6717.8(37)
_cod_database_code               4077806