Synthesis and reactivity of ruthenium tridentate bis-phosphinite ligand complexes.
Sgro, Michael J.; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 10460–10472; doi:10.1039/c3dt51065d

data_7021554
_publ_section_title
;
 Synthesis and reactivity of ruthenium tridentate bis-phosphinite ligand
 complexes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10460
_journal_page_last               10472
_journal_paper_doi               10.1039/c3dt51065d
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C34 H53 Cl N O2 P3 Ru'
_chemical_formula_weight         737.20
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.167(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.9644(8)
_cell_length_b                   17.3583(8)
_cell_length_c                   20.1248(9)
_cell_measurement_reflns_used    3317
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.07
_cell_measurement_theta_min      2.35
_cell_volume                     7672.8(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0699
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29264
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure   ! 
RESPONSE: During the 
refinement of the structure, electron density peaks were located 
that were believed to be highly disordered 
solvent molecules (possibly methylene chloride). Attempts 
made to model the solvent molecule were not successful. 
The SQUEEZE option in PLATON (Spek, 2009) indicated there was a 
large solvent cavity 1034.6 Ang^3. In the final cycles of refinement, 
this contribution (295) to the 
electron density was removed from the observed data. The 
density, the F(000) value, the molecular weight and the formula are 
given without taking into account the results obtained with the 
SQUEEZE option PLATON (Spek, 2009). Similar treatments of disordered 
solvent molecules were carried out by St\"ahler et al. (2001), 
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005). 
References: 
  
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
  
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005). 
Acta Cryst. E61, m2014-m2017. 
  
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M. 
(2003). Acta Cryst. E59, o975-o977. 
  
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M. 
(2003). Acta Cryst. C59, m84-m86. 
  
Stahler, R., Nather, C. & Bensch, W. (2001). Acta Cryst. 
C57, 26-27.
;
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         8769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                5894
_reflns_number_total             8769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51065d.txt
_cod_data_source_block           mjs047_Compound_6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7021554