In Vitro Evaluation of Rhodium and Osmium RAPTA Analogues: The Case for Organometallic Anticancer Drugs Not Based on Ruthenium
Dorcier, Antoine; Ang, Wee Han; Bolaño, Sandra; Gonsalvi, Luca; Juillerat-Jeannerat, Lucienne; Laurenczy, Gàbor; Peruzzini, Maurizio; Phillips, Andrew D.; Zanobini, Fabrizio; Dyson, Paul J.; Organometallics 25 (2006) 4090–; doi:10.1021/om060394o

data_4075600
_publ_section_title
;
 In Vitro Evaluation of Rhodium and Osmium RAPTA Analogues:&#x00A0; The
 Case for Organometallic Anticancer Drugs Not Based on Ruthenium
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4090
_journal_paper_doi               10.1021/om060394o
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C46.70 H61.81 B Cl N6 O0.705 P2 Rh'
_chemical_formula_sum            'C46.7 H61.81 B Cl N6 O0.705 P2 Rh'
_chemical_formula_weight         929.54
_chemical_name_common            'Cp*Rh(PTA)2Cl BPh4 MeOH'
_chemical_name_systematic
;
 Chloro-Pentamethylcyclodienyl-Bis-1,3,5-Triaza-7-phosphaadamantane-
 Rhodium(III) Tetraphenylborate with methanol solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.000
_cell_angle_beta                 107.800(7)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   11.9850(10)
_cell_length_b                   30.388(2)
_cell_length_c                   13.0020(9)
_cell_measurement_reflns_used    2321
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      32.3327
_cell_measurement_theta_min      4.3379
_cell_volume                     4508.6(6)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.pre23_10 beta (release 21.06.2004 CrysAlis171 .NET)
(compiled Jun 21 2004,12:00:08)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.pre23_10 beta (release 21.06.2004 CrysAlis171 .NET)
(compiled Jun 21 2004,12:00:08)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.pre23_10 beta (release 21.06.2004 CrysAlis171 .NET)
(compiled Jun 21 2004,12:00:08)
;
_computing_molecular_graphics    'ORTEPIII for Windows (Farrugia, 1997)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
  1 omega   -5.00  113.50   0.7500    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       35.0000   80.0000    0.0000    0.0000    0.0000 158

  2 omega   -5.00  113.50   0.7500    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       35.0000   80.0000  120.0000    0.0000    0.0000 158

  3 omega  -75.00   43.50   0.7500    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -35.0000   80.0000   90.0000    0.0000    0.0000 158

  4 phi   -180.00  169.50   0.7500    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
   0.0000   35.0000    0.0000     -        0.0000    0.0000 466

  5 omega   -8.00  112.00   0.7500    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       35.0000   40.0000   90.0000    0.0000    0.0000 160

  6 omega   -8.00  112.00   0.7500    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       35.0000   40.0000  120.0000    0.0000    0.0000 160

  7 omega  -78.00   42.00   0.7500    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -35.0000   40.0000   90.0000    0.0000    0.0000 160

  8 omega  -42.00   78.00   0.7500    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       35.0000  -40.0000   90.0000    0.0000    0.0000 160

  9 omega  -42.00   78.00   0.7500    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       35.0000  -40.0000  120.0000    0.0000    0.0000 160

 10 omega -112.00    8.00   0.7500    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -35.0000  -40.0000   90.0000    0.0000    0.0000 160

 11 omega  -44.00   74.50   0.7500    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       35.0000  -80.0000    0.0000    0.0000    0.0000 158

 12 omega  -44.00   74.50   0.7500    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       35.0000  -80.0000  120.0000    0.0000    0.0000 158
;
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      0.0092563078
_diffrn_orient_matrix_UB_12      0.0174153705
_diffrn_orient_matrix_UB_13      -0.0327731267
_diffrn_orient_matrix_UB_21      0.0543551839
_diffrn_orient_matrix_UB_22      -0.0094590533
_diffrn_orient_matrix_UB_23      0.0008115476
_diffrn_orient_matrix_UB_31      -0.0286910201
_diffrn_orient_matrix_UB_32      -0.0123306275
_diffrn_orient_matrix_UB_33      -0.0469908623
_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  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            101216
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         4.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.8016
_exptl_absorpt_correction_T_min  0.6732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2.03 (Bruker, 2001)
 [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1946
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.63
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+8.6896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                7960
_reflns_number_total             8037
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            om060394osi20060505_051727.cif
_cod_data_source_block           adp146
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C46.70 H61.81 B Cl N6 O0.705 P2 Rh'
_cod_database_code               4075600