Strategic Synthesis of [Cu2], [Cu4] and [Cu5] Complexes: Inhibition and Triggering of Ligand Arm Hydrolysis and Self-aggregation by Chosen Ancillary Bridges
Das, Manisha; Canaj, Angelos; Bertolasi, Valerio; Murrie, Mark; Ray, Debashis; Dalton Transactions  (2018) –; doi:10.1039/C8DT03390K

data_7048033
_publ_section_title
;
 Strategic Synthesis of [Cu2], [Cu4] and [Cu5] Complexes: Inhibition and
 Triggering of Ligand Arm Hydrolysis and Self-aggregation by Chosen
 Ancillary Bridges
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT03390K
_journal_year                    2018
_chemical_formula_moiety         '3(C24 H24 Cu2 N2 O4), 6(Cl O4), 4(H2 O)'
_chemical_formula_sum            'C72 H80 Cl6 Cu6 N6 O40'
_chemical_formula_weight         2263.36
_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   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2018-11-08 deposited with the CCDC.
2018-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                77.244(2)
_cell_angle_beta                 75.5060(19)
_cell_angle_gamma                71.192(2)
_cell_formula_units_Z            1
_cell_length_a                   12.3517(4)
_cell_length_b                   14.1130(5)
_cell_length_c                   14.4440(5)
_cell_measurement_reflns_used    29155
_cell_measurement_temperature    295
_cell_measurement_theta_max      25.500
_cell_measurement_theta_min      3.368
_cell_volume                     2280.45(14)
_computing_cell_refinement       'Denzo SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'Denzo SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP III (Burnett & Johnson, 1996)'
_computing_publication_material
'SHELXL-2014/6 (Sheldrick, 2014), PARST (Nardelli, 1995), PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29155
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         3.368
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             1150
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.546
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         8399
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0760
_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^)+(0.1853P)^2^+0.3648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2285
_refine_ls_wR_factor_ref         0.2567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5928
_reflns_number_total             8399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03390k2.cif
_cod_data_source_block           Complex1
_cod_database_code               7048033
_shelxl_version_number           2014/6
_shelx_res_checksum              39984