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_7048032
_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         'C38 H34 Cu4 F12 N4 O11'
_chemical_formula_sum            'C38 H34 Cu4 F12 N4 O11'
_chemical_formula_weight         1204.85
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5200(5)
_cell_length_b                   12.5200(5)
_cell_length_c                   35.8306(8)
_cell_measurement_reflns_used    16627
_cell_measurement_temperature    295
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      3.28
_cell_volume                     5616.5(3)
_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    Diamond
_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      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.983
_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  0.0538
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            16627
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         3.276
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.583
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3058
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+1.9648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2200
_reflns_number_total             3058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03390k2.cif
_cod_data_source_block           Complex2
_cod_original_cell_volume        5616.5(5)
_cod_database_code               7048032
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All F(H,H) groups
 At 1.5 times of:
  All F(H,H,H) groups
2. Restrained distances
 C7-C8
 1.51 with sigma of 0.01
 C8-C9A = C8-C9B
 1.42 with sigma of 0.01
 C10-C11
 1.51 with sigma of 0.01
 C11-F1A \\sim C11-F2A \\sim C11-F3A \\sim C11-F1B \\sim C11-F2B \\sim C11-F3B
 with sigma of 0.01
 F1A-F2A \\sim F1A-F3A \\sim F2A-F3A
 with sigma of 0.01
 F1B-F2B \\sim F1B-F3B \\sim F2B-F3B
 with sigma of 0.01
3. Others
 Fixed Sof: C9A(0.5) H9AA(0.5) H9AB(0.5) C9B(0.5) F1A(0.5) F2A(0.5) F3A(0.5)
 F1B(0.5) F2B(0.5) F3B(0.5) H5A(0.5) H5B(0.5) H5C(0.5) H9BA(0.5) H9BB(0.5)
 Fixed X: O1(0) C1(0) C4(0) C5(0) O2(0) H5A(0.0298) H5B(0.04214) H5C(-
 0.071939) H9BA(-0.295361) H9BB(-0.40591)
 Fixed Y: O1(0.25) C1(0.25) C4(0.25) C5(0.25) O2(0.25) H5A(0.18413)
 H5B(0.308741) H5C(0.25713) H9BA(0.161741) H9BB(0.124001)
 Fixed Z: O2(0.62501) H5A(0.38917) H5B(0.38917) H5C(0.38917) H9BA(0.556709)
 H9BB(0.575529)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8)
4.c X=CH2 refined with riding coordinates:
 C9A(H9AA,H9AB)
;
_shelx_res_checksum              73562
_shelx_fab_checksum              47407