Cocrystallization of Mononuclear and Trinuclear Metallacycle Molecules from an Aqueous Mixed-Ligand Copper(II) Solution
El Bakkali, Hanan; Choquesillo-Lazarte, Duane; Domínguez-Martín, Alicia; Pérez-Toro, M. Inmaculada; Lezama, L.; González-Pérez, Josefa M.; Castiñeiras, Alfonso; Niclós-Gutiérrez, Juan; Crystal Growth & Design 14 (2014) 889–; doi:10.1021/cg4015898

data_4510096
_publ_section_title
;
 Cocrystallization of Mononuclear and Trinuclear Metallacycle Molecules
 from an Aqueous Mixed-Ligand Copper(II) Solution
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              889
_journal_paper_doi               10.1021/cg4015898
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety
'C57 H57 Cu3 N15 O12, 3(C19 H21 Cu N5 O5), 21(H2 O)'
_chemical_formula_sum            'C114 H162 Cu6 N30 O48'
_chemical_formula_weight         3101.97
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   20.852(3)
_cell_length_b                   20.852(3)
_cell_length_c                   56.734(19)
_cell_measurement_temperature    293(2)
_cell_volume                     21363(8)
_computing_cell_refinement       'SMART Software (Nonius, 1997)'
_computing_data_collection       'SMART Software (Nonius, 1997)'
_computing_data_reduction        'SAINT Software (Nonius, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'SMART CCD-1000'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0875
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_limit_l_min       -73
_diffrn_reflns_number            83200
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.246
_diffrn_reflns_theta_min         1.826
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       plate
_exptl_crystal_F_000             9684
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
C101 0.673 0.349 0.784 !       1.27 eA-3
Q102 0.936 0.375 0.892 !       1.14 eA-3
C103 0.734 0.381 0.875 !       1.05 eA-3
Q104 0.403 0.782 0.124 !       0.89 eA-3
Q105 0.329 0.828 0.050 !       0.82 eA-3
Q106 0.911 0.077 0.532 !       0.76 eA-3
Q107 0.842 0.995 0.617 !       0.76 eA-3
C108 1.001 0.998 0.480 !       0.74 eA-3
Q109 0.636 0.452 0.688 !       0.71 eA-3
Q110 0.519 0.193 0.683 !       0.70 eA-3
;
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         11233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0674
_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^)+(0.1097P)^2^+24.1774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1713
_refine_ls_wR_factor_ref         0.1953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7355
_reflns_number_total             11233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg4015898_si_002.cif
_cod_data_source_block           13jnac542_new
_cod_original_cell_volume        21363(9)
_cod_database_code               4510096
_shelx_estimated_absorpt_t_min   0.612
_shelx_estimated_absorpt_t_max   0.971