The formation of cis- and trans-[Ru(CN)2(CNtBu)4] by reductive cleavage of isocyanide ligands; isomer separation by supramolecular interactions with various solvents
Daniel Dönnecke; Wolfgang Imhof; Dalton Trans.  (2003) 2737–2744; doi:10.1039/b304199a

data_7013095
_publ_section_title
;
 The formation of cis- and trans-[Ru(CN)2(CNtBu)4] by reductive
 cleavage of isocyanide ligands; isomer separation by supramolecular
 interactions with various solvents
;
_journal_issue                   13
_journal_name_full               'Dalton Trans.'
_journal_page_first              2737
_journal_page_last               2744
_journal_paper_doi               10.1039/b304199a
_journal_year                    2003
_chemical_formula_sum            'C36 H60 N9 O2 Ru1.5'
_chemical_formula_weight         802.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.905(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.9630(7)
_cell_length_b                   9.4494(2)
_cell_length_c                   18.3389(4)
_cell_measurement_temperature    183(2)
_cell_volume                     4588.09(19)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    XP
_computing_publication_material  XP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       KAPPA-CCD
_diffrn_measurement_method       'phi-scan, omega-scan'
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16849
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.536
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       quader
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.189
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.053
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         10272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_obs          0.0507
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+2.8855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1317
_refine_ls_wR_factor_obs         0.1124
_reflns_number_observed          7341
_reflns_number_total             10277
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b304199a.txt
_cod_data_source_block           tt1770
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+2.8855P] 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^)+(0.0511P)^2^+2.8855P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4588.1(2)
_cod_original_sg_symbol_H-M      P2/c
_cod_original_formula_sum        'C36 H60 N9 O2 Ru1.50'
_cod_database_code               7013095