Syntheses, Characterization, and Reactivity of Diruthenium Hydrido Complexes
Wiltse, Heather R.; Johnson, Alyssa N.; Durand, Raphael J.; Brennessel, William; Chin, Robert M.; Organometallics 35 (2016) 1079–; doi:10.1021/acs.organomet.6b00067

data_4086457
_publ_section_title
;
 Syntheses, Characterization, and Reactivity of Diruthenium Hydrido
 Complexes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1079
_journal_paper_doi               10.1021/acs.organomet.6b00067
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C52 H67 N4 Ru2, C O3 F3 S, 2.5(C6 H6)'
_chemical_formula_sum            'C68 H82 F3 N4 O3 Ru2 S'
_chemical_formula_weight         1294.57
_chemical_name_common            unimc31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   38.385(4)
_cell_length_b                   40.031(4)
_cell_length_c                   16.3398(15)
_cell_measurement_reflns_used    3945
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      34.62
_cell_measurement_theta_min      2.53
_cell_volume                     25108(4)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       63
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       66
_diffrn_reflns_limit_k_min       -66
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            144900
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        36.319
_diffrn_reflns_theta_max         36.360
_diffrn_reflns_theta_min         2.035
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       plate
_exptl_crystal_F_000             10768
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.398
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
; 
 Flack x determined using 7742 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.016(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         29710
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0491P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    0.956
_reflns_Friedel_fraction_max     0.953
_reflns_number_gt                21423
_reflns_number_total             29710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00067_si_002.cif
_cod_data_source_block           unimc31
_cod_depositor_comments
'Adding full bibliography for 4086455--4086457.cif.'
_cod_original_cell_volume        25107(4)
_cod_database_code               4086457
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.856
_shelx_estimated_absorpt_t_max   0.914
_shelx_res_checksum              9309
_shelx_hkl_checksum              84103