Diruthenium(III,III) Bis(alkynyl) Compounds with Donor/Acceptor-Substituted geminal-Diethynylethene Ligands
William P. Forrest; Zhi Cao; Kerry M. Hassell; Boone M. Prentice; Phillip E. Fanwick; Tong Ren; Inorganic Chemistry 51 (2012) 3261–3269; doi:10.1021/ic202720c

data_4328586
_publ_contact_author_address
;    Department of Chemistry
     Purdue University
     560 Oval Dr.
     W. Lafayette
     IN 47907-2084
     USA
;
_publ_contact_author_email       pfanwick@purdue.edu
_publ_contact_author_fax         1(765)4940239
_publ_contact_author_name        'Fanwick, Phillip E.'
_publ_contact_author_phone       1(765)4944572
_publ_section_title
;
 Diruthenium(III,III) Bis(alkynyl) Compounds with
 Donor/Acceptor-Substituted geminal-Diethynylethene Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3261
_journal_page_last               3269
_journal_paper_doi               10.1021/ic202720c
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C70 H98 N8 Ru2 Si2,C4 H8 O1'
_chemical_formula_sum            'C74 H106 N8 O Ru2 Si2'
_chemical_formula_weight         1382.03
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                80.515(8)
_cell_angle_beta                 79.918(10)
_cell_angle_gamma                87.793(12)
_cell_formula_units_Z            2
_cell_length_a                   10.6263(15)
_cell_length_b                   16.654(3)
_cell_length_c                   21.360(3)
_cell_measurement_reflns_used    12202
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      67
_cell_measurement_theta_min      2
_cell_volume                     3670.7(10)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_collection       'CrystalClear(Rigaku, 2001)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
    ORTEP (Johnson, 1976)
    PLATON (Spek, 2003)
;
_computing_publication_material  'SHELX97(Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_structure_solution
;
 direct methods (SIR2004, Burla et al., 2005)
;
_diffrn_ambient_temperature      150.0(2)
_diffrn_measured_fraction_theta_full 0.9690
_diffrn_measured_fraction_theta_max 0.9690
_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 HKL2000/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_monochromator  'confocal optics'
_diffrn_radiation_type           CU-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58683
_diffrn_reflns_theta_full        55.0
_diffrn_reflns_theta_max         67.11
_diffrn_reflns_theta_min         2.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.071
_exptl_absorpt_correction_T_max  0.9218
_exptl_absorpt_correction_T_min  0.5730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       plate
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_platon_squeeze_details
'                                                                       '
_refine_diff_density_max         1.62
_refine_diff_density_min         -0.75
_refine_ls_d_res_high            0.93
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         9274
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.099
_refine_ls_R_factor_gt           0.078
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1514P)^2^+4.1812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.218
_refine_ls_wR_factor_ref         0.234
_reflns_number_gt                7210
_reflns_number_total             9274
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            ic202720c_si_001_2.cif
_cod_data_source_block           WF792
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
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 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_formula_sum        'C74 H106 N8 O1 Ru2 Si2'
_cod_database_code               4328586