Ruthenium Assisted Reversible Proton Transfer from an Aromatic Carbon to a Hydride
Andrew J. Toner; Stephan Gründemann; Eric Clot; Hans-Heinrich Limbach; Bruno Donnadieu; Sylviane Sabo-Etienne; Bruno Chaudret; Journal of the American Chemical Society 122 (2000) 6777–6778; doi:10.1021/ja9943997

data_4116091
_publ_contact_author             B.Chaudret
_publ_contact_author_email       chaudret@lcctoul.lcc-toulouse.fr
_publ_section_title
;
 Ruthenium Assisted Reversible Proton Transfer from an Aromatic Carbon to
 a Hydride
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6777
_journal_page_last               6778
_journal_paper_doi               10.1021/ja9943997
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C65 H74 B F24 N O P2 Ru'
_chemical_formula_weight         1515.07
_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
_cell_angle_beta                 110.70(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.232(3)
_cell_length_b                   25.028(5)
_cell_length_c                   19.142(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      52.0
_cell_measurement_theta_min      4.1
_cell_volume                     6826(3)
_computing_cell_refinement
;
Stoe and Cie (1996) IPDS Manual. 
Version 2.75. Stoe and Cie, Darmstadt, Germany
;
_computing_data_collection
;
Stoe and Cie (1996) IPDS Manual. 
Version 2.75. Stoe and Cie, Darmstadt, Germany
;
_computing_data_reduction
;
Stoe and Cie (1996) IPDS Manual. 
Version 2.75. Stoe and Cie, Darmstadt, Germany
;
_computing_molecular_graphics
;
Zsolnai,L.(1997). ZORTEP.Molecular Graphics 
Program.University of Heidelberg, Germany
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
Altomare, A., Cascarano, G., Giacovazzo G., 
Guagliardi A., Burla M.C., Polidori, G.  & Camalli, M. (1994) SIR92 - a 
program for automatic solution of crystal structures by direct methods.
 J. Appl. Cryst. (27), 435
;
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type
;
Stoe and Cie (1996) IPDS Manual. 
Version 2.75. Stoe and Cie, Darmstadt, Germany
;
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39875
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
numerical corrections absorption (X-SHAPE 
Crystal Optimisation for numerical Absorption Correction Revision 1.01 July 
1996 STOE and Cie 1996) were applied on the data by using a set of symmetry 
equivalent reflections selected with the criterion [I/?(I)>30] such that all 
directions are equally represented. Starting from an initial crystal 
description, the program applies numerical absorption correction to the set 
of symmetry equivalent reflection and calculates the merging R-factor R(int). 
This is repeated until to reach a minima for R(int).
;
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         9389
_refine_ls_number_restraints     595
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.743
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+7.5913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                8414
_reflns_number_total             9389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9943997.cif
_cod_data_source_block           C65H74BF24NOP2Ru
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        6826(2)
_cod_database_code               4116091