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_4343440
_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_moiety
'C96 H129 B2 Cu12 N14 O28, 4(B F4), 4(H2 O), 12(C3 H7 N O), 8(C2 H6 O)'
_chemical_formula_sum            'C148 H269 B6 Cu12 F16 N26 O52'
_chemical_formula_weight         4376.22
_chemical_name_common
'[Cu6BO3(L)(OH)(DMF)(H20)3]2[BF4]2*12(DMF)*8(EtOH)*4(H2O) (3)'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.255(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.740(5)
_cell_length_b                   15.232(2)
_cell_length_c                   33.008(4)
_cell_measurement_reflns_used    4017
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.19
_cell_measurement_theta_min      2.31
_cell_volume                     16247(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1117
_diffrn_reflns_av_unetI/netI     0.1096
_diffrn_reflns_laue_measured_fraction_full 0.979
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            64065
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         1.250
_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             9136
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
The solvent electron density was modeled using 5599.2 \%A3 and an
electron count of 2974 electrons/cell, consistent with 48 DMF moelcules,
16 waters and 32 ethanol molecules/cell.  These additional molecules
were added to the contents of the unit cell during the final refinement
to properly calculate the crystal data. 
;
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         14400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.664
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.1772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7855
_reflns_number_total             14400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00771_si_002.cif
_cod_data_source_block           three
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4343438--4343442.cif.
;
_cod_database_code               4343440
_shelx_estimated_absorpt_t_min   0.683
_shelx_estimated_absorpt_t_max   0.852
_shelxl_version_number           2013-3
_shelx_res_checksum              36786
_shelx_hkl_checksum              12830