Enhancement of the antiproliferative activity of [RuCp(PPh3)2(dmoPTA-1κP)]+ via its coordination to one {CoCl2} unit: synthesis, crystal structure and properties of [RuCp(PPh3)2-μ-dmoPTA-1κP:2κ2N,N’-CoCl2](OTf)·0.25H2O.
Mendoza, Zenaida; Lorenzo-Luis, Pablo; Scalambra, Franco; Padrón, José M.; Romerosa, Antonio; Dalton Trans.  (2017) –; doi:10.1039/C7DT01741C

data_7043166
_publ_section_title
;
 Enhancement of the antiproliferative activity of
 [RuCp(PPh3)2(dmoPTA-1\kP)]+ via its coordination to one {CoCl2} unit:
 synthesis, crystal structure and properties of
 [RuCp(PPh3)2-\m-dmoPTA-1\kP:2\k2N,N&#x2019;-CoCl2](OTf)&#x00B7;0.25H2O.
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01741C
_journal_year                    2017
_chemical_formula_moiety         'C48 H51 Cl2 Co N3 P3 Ru, C F3 O3 S, 0.25(O)'
_chemical_formula_sum            'C49 H53 Cl2 Co F3 N3 O3.25 P3 Ru S'
_chemical_formula_weight         1148.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-26
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.05.22 svn.r3414 for OlexSys, GUI svn.r5347)
;
_audit_update_record
;
2017-05-26 deposited with the CCDC.
2017-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                106.3010(10)
_cell_angle_beta                 93.3240(10)
_cell_angle_gamma                94.3000(10)
_cell_formula_units_Z            4
_cell_length_a                   11.1351(8)
_cell_length_b                   20.8269(15)
_cell_length_c                   22.1074(16)
_cell_measurement_reflns_used    9209
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.78
_cell_measurement_theta_min      2.18
_cell_volume                     4890.2(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28770
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.804
_diffrn_reflns_theta_min         0.963
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.3776
_exptl_absorpt_correction_T_min  0.3377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0489 before and 0.0307 after correction. The Ratio of minimum to maximum transmission is 0.8943. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.041
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1212
_refine_ls_number_reflns         19829
_refine_ls_number_restraints     1243
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0443P)^2^+9.9711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17138
_reflns_number_total             19829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01741c2.cif
_cod_data_source_block           zm381m_0m
_cod_database_code               7043166
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Co1-Cl2 \\sim Co1-Cl3
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Cl3)=1-FVAR(1)
 Sof(Cl2)=FVAR(1)
 Sof(O1AA)=0.5*(1-FVAR(3))
 Sof(O0AA)=0.5*FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C44A(H44C,H44D), C44(H44A,H44B), C43A(H43C,H43D), C43(H43A,H43B), C42(H42A,
 H42B), C45A(H45C,H45D), C42A(H42C,H42D), C46(H46A,H46B), C46A(H46C,H46D),
 C45(H45A,H45B)
5.b Aromatic/amide H refined with riding coordinates:
 C18A(H18A), C17A(H17A), C18(H18), C17(H17), C35A(H35A), C34A(H34A),
 C26A(H26A), C36A(H36A), C24A(H24A), C41A(H41A), C38A(H38A), C33A(H33A),
 C24(H24), C3(H3), C30A(H30A), C37A(H37A), C32(H32), C20A(H20A), C38(H38),
 C27A(H27A), C2A(H2A), C23(H23), C5(H5), C39A(H39A), C9(H9), C37(H37),
 C29A(H29A), C2(H2), C15(H15), C16(H16), C14(H14), C12A(H12A), C36(H36),
 C39(H39), C40A(H40A), C14A(H14A), C26(H26), C32A(H32A), C20(H20), C21A(H21A),
 C16A(H16A), C12(H12), C8(H8), C4(H4), C6(H6), C30(H30), C33(H33), C21(H21),
 C22A(H22A), C11(H11), C28A(H28A), C10(H10), C41(H41), C15A(H15A), C34(H34),
 C3A(H3A), C35(H35), C8A(H8A), C22(H22), C29(H29), C40(H40), C11A(H11A),
 C23A(H23A), C9A(H9A), C6A(H6A), C27(H27), C10A(H10A), C28(H28), C4A(H4A),
 C5A(H5A)
5.c Idealised Me refined as rotating group:
 C48A(H48D,H48E,H48F), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C47A(H47D,
 H47E,H47F)
;
_olex2_submission_special_instructions 'No special instructions were received'