Facile Modification of 1,3,5-Triaza-7-phosphatricyclo[3.3.1.13,7]decane Phosphanes Coordinated to Ruthenium(II)
Almudena García-Fernández; Josefina Díez; M. Pilar Gamasa; Elena Lastra; Inorganic Chemistry 48 (2009) 2471–2481; doi:10.1021/ic801710y

data_4301664
_publ_contact_author
;     Josefina D\'iez
      Departamento de Qu\'imica Org\'anica e Inorg\'anica
      Facultad de Qu\'imica
      Universidad de Oviedo
      Avda. Juli\'an Claver\'ia, 8
      33006 Oviedo
      Spain
;
_publ_contact_author_email       jdv@uniovi.es
_publ_contact_author_fax         '0034 98 5103446'
_publ_contact_author_phone       '0034 98 5102960'
_publ_section_title
;
Facile Modification of 1,3,5-Triaza-7-phosphatricyclo[3.3.1.13,7]decane
Phosphanes Coordinated to Ruthenium(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2471
_journal_page_last               2481
_journal_paper_doi               10.1021/ic801710y
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C33 H37 B Cl I2 N9 P2 Ru, 1/2(C H2 Cl2)'
_chemical_formula_sum            'C33.5 H38 B Cl2 I2 N9 P2 Ru'
_chemical_formula_weight         1065.25
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.407(3)
_cell_angle_beta                 92.830(3)
_cell_angle_gamma                100.590(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9698(3)
_cell_length_b                   10.8518(4)
_cell_length_c                   18.2308(6)
_cell_measurement_reflns_used    12541
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.8030
_cell_measurement_theta_min      4.1522
_cell_volume                     1929.01(11)
_computing_cell_refinement
;
CrysAlisPro RED (Oxford Diffraction, 2008)
;
_computing_data_collection
;
CrysAlisPro CCD (Oxford Diffraction, 2008)
;
_computing_data_reduction
;
CrysAlisPro RED (Oxford Diffraction, 2008)
;
_computing_molecular_graphics    'PLATON (Spek, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device
; 
165 mm Onyx CCD detector in \k-geometry diffractometer
;
_diffrn_measurement_device_type
;
 Oxford Diffraction Xcalibur Nova
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18045
_diffrn_reflns_theta_full        74.34
_diffrn_reflns_theta_max         74.34
_diffrn_reflns_theta_min         4.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.224
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlis RED, Oxford Diffraction Ltd.,
(Oxford Diffraction, 2008).
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1038
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.186
_refine_diff_density_min         -1.637
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         7392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0784p)^2^+14.8638p] where p=(fo^2^+2fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1564
_reflns_number_gt                6383
_reflns_number_total             7392
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            ic801710y_si_001_2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_structure_factor_coef' value 'fsqd' changed to
'Fsqd' 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 
;
_cod_original_formula_sum        'C33.50 H38 B Cl2 I2 N9 P2 Ru'
_cod_database_code               4301664