Synthesis and Characterization of the Series of Compounds Ru2(O2CMe)x(admp)4-xCl (Hadmp = 2-Amino-4,6-dimethylpyridine, x = 3, 2, 1, 0)
F. A. Cotton; A. Yokochi; Inorganic Chemistry 37 (1998) 2723–2728; doi:10.1021/ic971428a

data_4322814
_publ_section_title
;
 Synthesis and Characterization of the Series of Compounds
 Ru2(O2CMe)x(admp)4-xCl (Hadmp = 2-Amino-4,6-dimethylpyridine, x = 3, 2,
 1, 0)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2723
_journal_page_last               2728
_journal_paper_doi               10.1021/ic971428a
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        synthesis
_chemical_formula_moiety         'Ru2 Cl (C7H9N2)3 (O2CCH3), C7H10N2, C6H6'
_chemical_formula_structural
'RU2(HNC5H2N(CH3)2)3(O2CCH3)CL (H2NC5H2N(CH3)2) (C6H6)'
_chemical_formula_sum            'C36 H46 Cl N8 O2 Ru2'
_chemical_formula_weight         860.40
_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                 109.211(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.979(2)
_cell_length_b                   14.9294(14)
_cell_length_c                   17.131(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      8.9
_cell_volume                     3859.1(11)
_computing_cell_refinement       Madnes
_computing_data_collection       Madnes
_computing_data_reduction        Absurd
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid mask fitting'
_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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0949
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12745
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.53
_diffrn_standards_interval_count None
_diffrn_standards_interval_time  None
_diffrn_standards_number         None
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_T_max  0.847(8)
_exptl_absorpt_correction_T_min  0.669(10)
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.132
_refine_ls_goodness_of_fit_obs   1.204
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         4294
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.122
_refine_ls_restrained_S_obs      1.191
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_obs          0.0682
_refine_ls_shift/esd_max         -0.055
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+13.5121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1619
_refine_ls_wR_factor_obs         0.1501
_reflns_number_observed          3363
_reflns_number_total             4294
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971428a_3.cif
_cod_data_source_block           cmpd_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'Noref' changed to 'noref'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'None' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+13.5121P] 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^)+(0.0418P)^2^+13.5121P] 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        3859.0(12)
_cod_database_code               4322814