Isonitrile Insertion into the Ru−O Bond and Migratory C−C Bond Formation. Novel Organoruthenium Imidic Ester and Acyl Species
Panda, Bikash Kumar; Chattopadhyay, Swarup; Ghosh, Kaushik; Chakravorty, Animesh; Organometallics 21 (2002) 2773–; doi:10.1021/om020059+

data_4084040
_publ_section_title
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 Isonitrile Insertion into the Ru&#x2212;O Bond and Migratory C&#x2212;C
 Bond Formation. Novel Organoruthenium Imidic Ester and Acyl Species
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_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2773
_journal_paper_doi               10.1021/om020059+
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C64 H66 Cl5 N3 O2 P2 Ru'
_chemical_formula_weight         1249.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.902(5)
_cell_length_b                   20.570(7)
_cell_length_c                   21.407(7)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     6562(4)
_computing_cell_refinement       'Siemens P3/P4-PC V4.27'
_computing_data_collection       'Siemens P3/P4-PC V4.27'
_computing_data_reduction        'Siemens P3/P4-PC V4.27'
_computing_molecular_graphics    'Siemens SHELXTL V5.03 PC'
_computing_publication_material  'Siemens SHELXTL V5.03 PC'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       '\w scans'
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5719
_diffrn_reflns_theta_max         24.05
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       Parallelopiped
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.043
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     694
_refine_ls_number_reflns         5624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.324
_refine_ls_restrained_S_obs      1.043
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_obs          0.0662
_refine_ls_shift/esd_max         0.279
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1120P)^2^+10.0639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2597
_refine_ls_wR_factor_obs         0.1639
_reflns_number_observed          3785
_reflns_number_total             5636
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om020059%2B.cif
_cod_data_source_block           630ru
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1120P)^2^+10.0639P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1120P)^2^+10.0639P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Heavy atom method' was changed
to 'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        6562.0(38)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4084040