Esterification of the free carboxylic group from the lutidinic acid ligand as a tool to improve the cytotoxicity of Ru(ii) complexes
Honorato, João; Colina-Vegas, Legna; Correa, Rodrigo S.; Guedes, Adriana P. M.; Miyata, Marcelo; Pavan, Fernando R.; Ellena, Javier; Batista, Alzir A.; Inorganic Chemistry Frontiers 6 (2019) 376–; doi:10.1039/C8QI00941D

data_4349915
_publ_section_title
;
 Esterification of the free carboxylic group from the lutidinic acid
 ligand as a tool to improve the cytotoxicity of Ru(ii) complexes
;
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              376
_journal_paper_doi               10.1039/C8QI00941D
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C45 H40 N3 O4 P2 Ru, F6 P'
_chemical_formula_sum            'C45 H40 F6 N3 O4 P3 Ru'
_chemical_formula_weight         994.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-09 deposited with the CCDC.
2018-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.496(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.71(2)
_cell_length_b                   15.001(9)
_cell_length_c                   14.658(9)
_cell_measurement_reflns_used    10502
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.40
_cell_volume                     8910(9)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_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      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39913
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.380
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       prism
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         10186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+12.4458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8207
_reflns_number_total             10186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00941d2.cif
_cod_data_source_block           cb24
_cod_database_code               4349915
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.874
_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 O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3A) = Uanis(O3B)
3. Others
 Fixed Sof: O3A(0.5) O3B(0.5)
4.a Riding coordinates:
 O4(H4)
4.b Secondary CH2 refined with riding coordinates:
 C131(H13A,H13B), C132(H13C,H13D), C231(H23A,H23B), C232(H23C,H23D)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4A), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C112(H112), C113(H113), C114(H114), C115(H115), C116(H116),
  C122(H122), C123(H123), C124(H124), C125(H125), C126(H126), C212(H212),
 C213(H213), C214(H214), C215(H215), C216(H216), C222(H222), C223(H223),
 C224(H224), C225(H225), C226(H226)
;
_olex2_submission_special_instructions 'No special instructions were received'