Rational Design of Selective Organoruthenium Inhibitors of Protein Tyrosine Phosphatase 1B
Jun Xiang Ong; Chun Wei Yap; Wee Han Ang; Inorganic Chemistry 51 (2012) 12483–12492; doi:10.1021/ic301884j

data_4331087
_publ_contact_author_address
;National University of Singapore
Department of Chemistry
Block S15, Level 5
3 Science Drive 2
Singapore 117543
;
_publ_contact_author_email       chmawh@nus.edu.sg
_publ_contact_author_fax         '+65-6779 1691'
_publ_contact_author_name        'Wee Han Ang'
_publ_contact_author_phone       '+65-6516 5131'
_publ_section_title
;
 Rational Design of Selective Organoruthenium Inhibitors of Protein
 Tyrosine Phosphatase 1B
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12483
_journal_page_last               12492
_journal_paper_doi               10.1021/ic301884j
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C30 H29 Cl F2 N3 O3 P Ru, 4(C H4 O)'
_chemical_formula_sum            'C34 H45 Cl F2 N3 O7 P Ru'
_chemical_formula_weight         813.22
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                101.457(4)
_cell_angle_beta                 101.362(4)
_cell_angle_gamma                92.915(4)
_cell_formula_units_Z            2
_cell_length_a                   10.653(3)
_cell_length_b                   12.504(3)
_cell_length_c                   14.449(4)
_cell_measurement_reflns_used    3256
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      2.19
_cell_volume                     1841.2(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0782
_diffrn_reflns_av_sigmaI/netI    0.0911
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23737
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.4311
_exptl_absorpt_correction_T_min  0.3062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2008)'
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_meas      ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.767
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8442
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0592P)^2^+4.5399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                6647
_reflns_number_total             8442
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301884j_si_002_1.cif
_cod_data_source_block           c163
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not Measured' 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        1841.3(8)
_cod_database_code               4331087