Synthesis and Antiproliferative Activity of [RuCp(PPh3)2(HdmoPTA)](OSO2CF3)2 (HdmoPTA = 3,7-H-3,7-Dimethyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane).
Mendoza, Zenaida; Lorenzo-Luis, Pablo; Serrano-Ruiz, Manuel; Martín-Batista, Elva; Padrón, José M; Scalambra, Franco; Romerosa, Antonio; Inorganic chemistry 55 (2016) 7820–7822; doi:10.1021/acs.inorgchem.6b01207

data_4348481
_publ_section_title
;
 Synthesis and Antiproliferative Activity of
 [RuCp(PPh3)2(HdmoPTA)](OSO2CF3)2 (HdmoPTA =
 3,7-H-3,7-Dimethyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane).
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7820
_journal_page_last               7822
_journal_paper_doi               10.1021/acs.inorgchem.6b01207
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C48 H52 N3 P3 Ru, 2(C F3 O3 S)'
_chemical_formula_sum            'C50 H52 F6 N3 O6 P3 Ru S2'
_chemical_formula_weight         1163.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.7722(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2838(2)
_cell_length_b                   15.0822(3)
_cell_length_c                   30.4789(6)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      66.869
_cell_measurement_theta_min      2.934
_cell_volume                     5126.36(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker D8 VENTURE'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.7
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.915
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            17950
_diffrn_reflns_point_group_measured_fraction_full 0.915
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        66.922
_diffrn_reflns_theta_max         66.922
_diffrn_reflns_theta_min         3.277
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.755
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.073
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.842
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0713P)^2^+10.3343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7095
_reflns_number_total             8362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01207_si_002.cif
_cod_data_source_block           1_1
_cod_database_code               4348481
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: S11T(0.5) S12T(0.5) F21T(0.26) F22T(0.17) F23T(0.6) F24T(0.51)
 F25T(0.45) F26T(0.67) F27T(0.34) O21T(0.31) O22T(0.1) O23T(0.3) O24T(0.6)
 O25T(0.47) O26T(0.75) O27T(0.26) O28T(0.21) C1(0.5) C11T(0.5)
3.a Ternary CH refined with riding coordinates:
 N71(H71)
3.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C75(H75A,H75B), C76(H76A,H76B)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66),
  C81(H81), C82(H82), C83(H83), C84(H84), C85(H85)
3.d Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C77(H77A,H77B,H77C)
;
_shelx_res_checksum              55324
_shelx_hkl_checksum              90955
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'