Phenyl substituted indenylphosphine ruthenium complexes as catalysts for dehydrogenation of alcohols.
Yuan, Jia; Sun, Yue; Yu, Guang-Ao; Zhao, Cui; She, Neng-Fang; Mao, Shu-Lan; Huang, Peng-Shou; Han, Zhi-Jun; Yin, Jun; Liu, Sheng-Hua; Dalton transactions (Cambridge, England : 2003) 41 (2012) 10309–10316; doi:10.1039/c2dt30499f

data_7030269
_publ_section_title
;
 Phenyl substituted indenylphosphine ruthenium complexes as catalysts for
 dehydrogenation of alcohols.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10309
_journal_page_last               10316
_journal_paper_doi               10.1039/c2dt30499f
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C27 H33 Cl2 P Ru'
_chemical_formula_sum            'C27 H33 Cl2 P Ru'
_chemical_formula_weight         560.47
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.814(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.7462(13)
_cell_length_b                   9.5164(7)
_cell_length_c                   36.246(3)
_cell_measurement_reflns_used    6676
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.21
_cell_volume                     5769.3(8)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10128
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Single crystal of 8(H\~2\~O)\~2\~ suitable for X-ray diffraction was grown from
the anhydrous CH\~2\~Cl\~2\~. The intensity of 1012 is independent reflection.
Single crystal of 8(H\~2\~O)\~2\~ suitable for X-ray diffraction was grown
from the anhydrous CH\~2\~Cl\~2\~. The intensity of 1012 is independent
reflection. with I >2delta(I) were measured on a Bruker Smart Apex CCD
area-detector diffractometer with Mo-K\a radiation (\l = 0.71073 ?). The
structure was solved by direct methods and refined on F2 using SHELXL-97.
Owing to the seriously disorder, unsolved solvent molecules, the contribution
of the solvent molecules to the diffraction pattern was subtracted using the
SQUEEZE procedure of PLATON. The result indicated that the solvent-accessible
void in the unit cell has a volume of 1127.3 ?3 (consisting of about 19.5% of
the crystal volume, equally distributed across two cavities). The residual
electron density count amounted to 170 e per unit cell, corresponding to
nearly 16 molecules of H~2~O (the content of each of the two cavities per unit
cell being equivalent about 8 molecules of H~2~O, i.e. every molecule of 8
being distributed with 2 water molecules.) Crystal data for 8:
C~27~H~33~Cl~2~PRu, Mr = 560.47, Monoclinic, space group P21/n, a =
16.7462(13), b =9.5164(7), c = 36.246(3) ?, Z = 8, V = 5769.3(8)?3, Dc =
1.291g.cm-3, \m = 0.796 mm-1, \qmax = 28.28, F(000) = 2304, reflections
collected/unique, 10128/10128 (Rint = 0.0000), final R indices [I >2delta(I)]
R1 = 0.0909, wR2 = 0.1834, R indices (all data) R1 = 0.0971, wR2 = 0.1862, GOF
= 1.279 for all data.
;
_refine_diff_density_max         2.068
_refine_diff_density_min         -1.530
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.279
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         10128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.279
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0909
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+32.9473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1834
_refine_ls_wR_factor_ref         0.1862
_reflns_number_gt                9397
_reflns_number_total             10128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30499f.txt
_cod_data_source_block           110629em
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7030269