Synthesis and Electronic Structure of Ru2(Xap)4(Y-gem-DEE) Type Compounds: Effect of Cross-Conjugation.
Forrest, William P.; Choudhuri, Mohommad M. R.; Kilyanek, Stefan M.; Natoli, Sean N.; Prentice, Boone M.; Fanwick, Phillip E.; Crutchley, Robert J.; Ren, Tong; Inorganic chemistry 54 (2015) 7645–7652; doi:10.1021/acs.inorgchem.5b01315

data_4346345
_publ_section_title
;
 Synthesis and Electronic Structure of Ru2(Xap)4(Y-gem-DEE) Type
 Compounds: Effect of Cross-Conjugation.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7645
_journal_page_last               7652
_journal_paper_doi               10.1021/acs.inorgchem.5b01315
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C52 H43 N8 Ru2,C5 H12'
_chemical_formula_sum            'C57 H55 N8 Ru2'
_chemical_formula_weight         1054.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                100.918(10)
_cell_angle_beta                 93.269(14)
_cell_angle_gamma                93.815(13)
_cell_formula_units_Z            2
_cell_length_a                   9.9793(17)
_cell_length_b                   13.587(2)
_cell_length_c                   18.825(3)
_cell_measurement_reflns_used    34915
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      59.118
_cell_measurement_theta_min      3.702
_cell_volume                     2494.4(7)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'DIRDIF/PATTY (Burskens, et. al,. 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL3000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.102
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34915
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        59.118
_diffrn_reflns_theta_max         59.118
_diffrn_reflns_theta_min         3.702
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    5.255
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.410
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         6605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1558P)^2^+3.2860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2263
_refine_ls_wR_factor_ref         0.2579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4269
_reflns_number_total             6605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01315_si_002.cif
_cod_data_source_block           WF91C
_cod_original_cell_volume        2494.4(8)
_cod_database_code               4346345
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.420
_shelx_estimated_absorpt_t_max   0.949
_shelx_res_checksum              78023
_shelx_hkl_checksum              40243