Antiferromagnetically Coupled Dimeric Dodecacopper Supramolecular Architectures of Macrocyclic Ligands with a Symmetrical μ6-BO3(3-) Central Moiety.
Tandon, Santokh S.; Bunge, Scott D.; Toth, Sara A.; Sanchiz, Joaquin; Thompson, Laurence K.; Shelley, Jacob T.; Inorganic chemistry 54 (2015) 6873–6884; doi:10.1021/acs.inorgchem.5b00771

data_4343441
_publ_section_title
;
 Antiferromagnetically Coupled Dimeric Dodecacopper Supramolecular
 Architectures of Macrocyclic Ligands with a Symmetrical \m6-BO3(3-)
 Central Moiety.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6873
_journal_page_last               6884
_journal_paper_doi               10.1021/acs.inorgchem.5b00771
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C124 H264 B4 Cu12 F8 N12 O68'
_chemical_formula_weight         3969.18
_chemical_name_common
'[Cu6L(BO3)OAc(OMe)HOMe]2[BF4]216H2O26CH3OH (5)'
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.849(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.9843(18)
_cell_length_b                   14.7739(18)
_cell_length_c                   33.108(4)
_cell_measurement_reflns_used    8905
_cell_measurement_temperature    189(2)
_cell_measurement_theta_max      23.67
_cell_measurement_theta_min      2.18
_cell_volume                     7221.3(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      189(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_laue_measured_fraction_full 0.978
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            57289
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         1.248
_exptl_absorpt_coefficient_mu    1.845
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_platon_squeeze_details
; 
 The solvent electron density was modeled using 2869.7 \%A3 
 and an electron count of 1271 electrons/cell,consistent with 
 32 water and 52 methanol molecules/cell.  32 water molecules 
 and 52 methanol molecules were added to the contents of the 
 unit cell during the final refinement to properly calculate the crystal data. 
;
_refine_diff_density_max         1.170
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         12777
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          1.935
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.1962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1849
_refine_ls_wR_factor_ref         0.1936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8445
_reflns_number_total             12777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00771_si_002.cif
_cod_data_source_block           five
_cod_depositor_comments
'Adding full bibliography for 4343438--4343442.cif.'
_cod_original_cell_volume        7221.4(15)
_cod_database_code               4343441
_shelx_estimated_absorpt_t_min   0.655
_shelx_estimated_absorpt_t_max   0.837
_shelxl_version_number           2013-3
_shelx_res_checksum              70172
_shelx_hkl_checksum              72135