X-ray Diffraction and NMR Studies on a Series of Binap-Based Ru(II) Hydroxyphosphine π-Arene Complexes
Tilmann J. Geldbach; Frank Breher; Volker Gramlich; P. G. Anil Kumar; Paul S. Pregosin; Inorganic Chemistry 43 (2004) 1920–1928; doi:10.1021/ic0352147

data_4310734
_publ_section_title
;
 X-ray Diffraction and NMR Studies on a Series of Binap-Based Ru(II)
 Hydroxyphosphine \p-Arene Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1920
_journal_page_last               1928
_journal_paper_doi               10.1021/ic0352147
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C33 H26 F3 O6.5 P2 Ru S'
_chemical_formula_weight         778.61
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.92(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.422(3)
_cell_length_b                   14.972(3)
_cell_length_c                   14.869(3)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     3193.5(11)
_computing_cell_refinement       'STOE DIF4'
_computing_data_collection       'PICKER STOE DIF4'
_computing_data_reduction        'STOE REDU4'
_computing_molecular_graphics    SHELXLTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'PICKER 4-circle Stoe upgrade'
_diffrn_measurement_method       ' \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3278
_diffrn_reflns_theta_max         50.00
_diffrn_reflns_theta_min         4.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 120
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    6.098
_exptl_absorpt_correction_T_max  .60
_exptl_absorpt_correction_T_min  .53
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       prism
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.072
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         3278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_obs          0.0474
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+4.2464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1290
_refine_ls_wR_factor_obs         0.1063
_reflns_number_observed          2172
_reflns_number_total             3278
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0352147si20031216_102813.cif
_cod_data_source_block           tjg105a
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+4.2464P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+4.2464P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C33 H26 F3 O6.50 P2 Ru S'
_cod_database_code               4310734