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_4077807
_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            'C38 H33 Cl Mn N3 O4'
_chemical_formula_weight         686.06
_chemical_name_systematic
; 
1,1,1,1-tetracarbonyl-2,3-bis[2,6-(dimethylphenyl)imino]-3-(p-chlorobenzyl)
-4-(2,6-dimethylphenyl)-4-azamangancylopent-4-ene 
 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 99.888(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3169(5)
_cell_length_b                   19.6021(8)
_cell_length_c                   17.1131(8)
_cell_measurement_reflns_used    201
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      1.59
_cell_volume                     3409.4(3)
_computing_cell_refinement       'SMART v4.05'
_computing_data_collection       'SMART v4.05 (Siemens, 1995)'
_computing_data_reduction        'SAINT v4.05 (Siemens, 1995)'
_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      296(2)
_diffrn_measurement_device       'Siemens SMART 1K CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0957
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16370
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_correction_T_min  0.7663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Sheldrick, 1996'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1463
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0310P)^2^+1.1469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1269
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                3923
_reflns_number_total             7947
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9903644.cif
_cod_data_source_block           6
_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 2.4.2 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_database_code               4077807