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_7013091
_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            'C12 H19 Cl3 N3 Ru0.5'
_chemical_formula_weight         362.19
_chemical_name_systematic
;
?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.759(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2282(4)
_cell_length_b                   10.0166(4)
_cell_length_c                   17.6631(5)
_cell_measurement_temperature    183(2)
_cell_volume                     1749.91(11)
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6727
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.929
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       quader
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.092
_refine_ls_goodness_of_fit_obs   1.120
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_restrained_S_obs      1.120
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_obs          0.0308
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+0.9312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0750
_refine_ls_wR_factor_obs         0.0676
_reflns_number_observed          3174
_reflns_number_total             3914
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b304199a.txt
_cod_data_source_block           tt1648
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+0.9312P] 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^)+(0.0205P)^2^+0.9312P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C12 H19 Cl3 N3 Ru0.50'
_cod_database_code               7013091