Investigating the reactivity of neutral water-soluble Ru(ii)‒PTA carbonyls towards the model imine ligands pyridine and 2,2′-bipyridine
Battistin, Federica; Vidal, Alessio; Balducci, Gabriele; Alessio, Enzo; RSC Advances 10 (2020) 26717–26727; doi:10.1039/D0RA05898J

data_7240894
_publ_section_title
;
 Investigating the reactivity of neutral water-soluble Ru(ii)--PTA
 carbonyls towards the model imine ligands pyridine and
 2,2&#x2032;-bipyridine
;
_journal_issue                   45
_journal_name_full               'RSC Advances'
_journal_page_first              26717
_journal_page_last               26727
_journal_paper_doi               10.1039/D0RA05898J
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C18 H29 Cl2 N7 O P2 Ru'
_chemical_formula_sum            'C18 H29 Cl2 N7 O P2 Ru'
_chemical_formula_weight         593.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-06-04 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3610(12)
_cell_length_b                   16.8410(10)
_cell_length_c                   19.1660(15)
_cell_measurement_reflns_used    21605
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.088
_cell_measurement_theta_min      1.585
_cell_volume                     2375.9(5)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS - CCP4'
_computing_molecular_graphics
;
ShelXle (Hubschle et al. 2011)
Coot (Emsley et al., 2010) 
Ortep3 for Windows (Farrugia, 2012)
;
_computing_publication_material  'private software'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SHELXT (Sheldrick, 2015), Sir2014 (Burla, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type
;
Huber 4-circles Kappa Goniometer, Pilatus 2M detector
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0139
_diffrn_reflns_av_unetI/netI     0.0088
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48334
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         33.088
_diffrn_reflns_theta_min         1.585
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  1.258
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
        Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1208
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3/ether'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.280
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 3611 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.500(4)
_refine_ls_extinction_coef       0.0081(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         8401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+7.7609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1115
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.885
_reflns_number_gt                8337
_reflns_number_total             8401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra05898j2.cif
_cod_data_source_block           fb405-06
_cod_depositor_comments
'Adding full bibliography for 7240894--7240896.cif.'
_cod_database_code               7240894
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.756
_shelx_estimated_absorpt_t_max   0.908
_shelx_res_checksum              65606