Externally and Internally Functionalized Copper(II) β-Diketonate Molecular Squares.
Cherutoi, Jackson K.; Sandifer, Jace D.; Pokharel, Uttam R.; Fronczek, Frank R.; Pakhomova, Svetlana; Maverick, Andrew W.; Inorganic chemistry 54 (2015) 7791–7802; doi:10.1021/acs.inorgchem.5b00792

data_4346186
_publ_section_title
;
 Externally and Internally Functionalized Copper(II) \b-Diketonate
 Molecular Squares.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7791
_journal_page_last               7802
_journal_paper_doi               10.1021/acs.inorgchem.5b00792
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C128 H192 Cu4 O16, C70, 3.25(C6 H4 Cl2)'
_chemical_formula_sum            'C217.5 H205 Cl6.5 Cu4 O16'
_chemical_formula_weight         3559.39
_chemical_name_common
;
 tetrakis(m-phenylenebis(dihexanoylmethanato))-
 (mu-C70fullerene)tetracopper o-dichlorobenzene solvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                91.494(2)
_cell_angle_beta                 96.362(2)
_cell_angle_gamma                90.947(2)
_cell_formula_units_Z            4
_cell_length_a                   16.2905(8)
_cell_length_b                   21.8084(11)
_cell_length_c                   50.315(2)
_cell_measurement_reflns_used    9673
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      66.16
_cell_measurement_theta_min      4.01
_cell_volume                     17755.9(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Bruker Kappa APEX-II DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.915
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            126733
_diffrn_reflns_point_group_measured_fraction_full 0.665
_diffrn_reflns_point_group_measured_fraction_max 0.682
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.548
_diffrn_reflns_theta_min         2.027
_diffrn_source                   'I\mS microfocus'
_exptl_absorpt_coefficient_mu    1.960
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             7458
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.160
_refine_diff_density_max         5.214
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.229
_refine_ls_abs_structure_details
;
 Flack x determined using 19766 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.500(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.670
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7718
_refine_ls_number_reflns         85491
_refine_ls_number_restraints     22159
_refine_ls_restrained_S_all      2.696
_refine_ls_R_factor_all          0.1579
_refine_ls_R_factor_gt           0.1380
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3450
_refine_ls_wR_factor_ref         0.3738
_reflns_Friedel_coverage         0.453
_reflns_Friedel_fraction_full    0.415
_reflns_Friedel_fraction_max     0.425
_reflns_number_gt                70861
_reflns_number_total             85491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00792_si_002.cif
_cod_data_source_block           cpd27_JCheru22
_cod_original_cell_volume        17755.8(15)
_cod_database_code               4346186
_shelx_estimated_absorpt_t_min   0.640
_shelx_estimated_absorpt_t_max   0.744
_shelxl_version_number           2013-4
_shelx_res_checksum              57047
_shelx_hkl_checksum              25560
_shelx_fab_checksum              89687