Synthesis and characterization of five-coordinate, 16-electron Ru(II) complexes supported by tridentate bis(phosphino)silyl ligation.
MacInnis, Morgan C.; Ruddy, Adam J.; McDonald, Robert; Ferguson, Michael J.; Turculet, Laura; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15850–15858; doi:10.1039/c6dt01869f

data_7039454
_publ_section_title
;
 Synthesis and characterization of five-coordinate, 16-electron Ru(II)
 complexes supported by tridentate bis(phosphino)silyl ligation.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15850
_journal_page_last               15858
_journal_paper_doi               10.1039/c6dt01869f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C44.38 H75.5 P3 Ru Si'
_chemical_formula_weight         831.12
_chemical_name_systematic
; 
 ? 
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_IT_number           121
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2'
_symmetry_space_group_name_H-M   'I -4 2 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-15 deposited with the CCDC.
2016-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.5341(9)
_cell_length_b                   22.5341(9)
_cell_length_c                   17.3711(7)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.34
_cell_volume                     8820.8(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35591
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.9724
_exptl_absorpt_correction_T_min  0.8344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3558
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as disordered
or partial-occupancy solvent pentane carbon atoms were unsuccessful.
The data were corrected for disordered electron density through use of
the SQUEEZE procedure (Sluis, P. van der; Spek, A. L. Acta Crystallogr.
1990, A46, 194-201) as implemented in PLATON (Spek, A. L. Acta
Crystallogr. 1990, A46, C34; Spek, A. L. J. Appl. Cryst. 2003, 36, 7-13.
PLATON - a multipurpose crystallographic tool.  Utrecht University,
Utrecht, The Netherlands).  A total solvent-accessible void volume of
1229 cubic angstroms with a total electron count of 300 (consistent with
7 molecules of solvent pentane, or 0.875 molecules per formula unit of
the ruthenium complex) was found in the unit cell.
;
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         4722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0619
_reflns_number_gt                4371
_reflns_number_total             4722
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c6dt01869f2.cif
_cod_data_source_block           dal09d3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7039453--7039457.cif.
;
_cod_original_sg_symbol_H-M      I-42m
_cod_original_formula_sum        'C44.38 H75.50 P3 Ru Si'
_cod_database_code               7039454