Carving a 1D Co(II)-carboranylcarboxylate system by using organic solvents to create stable trinuclear molecular analogues: complete structural and magnetic studies.
Fontanet, Mònica; Rodríguez, Montserrat; Fontrodona, Xavier; Romero, Isabel; Teixidor, Francesc; Viñas, Clara; Aliaga-Alcalde, Núria; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10916–10927; doi:10.1039/c6dt01744d

data_7039417
_publ_section_title
;
 Carving a 1D Co(II)-carboranylcarboxylate system by using organic
 solvents to create stable trinuclear molecular analogues: complete
 structural and magnetic studies.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10916
_journal_page_last               10927
_journal_paper_doi               10.1039/c6dt01744d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C32 H106 B60 Co3 O18, 4 ( C4 H10 O )'
_chemical_formula_sum            'C48 H146 B60 Co3 O22'
_chemical_formula_weight         1901.03
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-04-01 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                63.006(12)
_cell_angle_beta                 73.533(13)
_cell_angle_gamma                67.443(11)
_cell_formula_units_Z            1
_cell_length_a                   14.420(9)
_cell_length_b                   14.806(10)
_cell_length_c                   15.656(10)
_cell_measurement_reflns_used    1449
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.84
_cell_measurement_theta_min      2.55
_cell_volume                     2726(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1692
_diffrn_reflns_av_unetI/netI     0.3208
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33699
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.215
_diffrn_reflns_theta_min         1.793
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.425520
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v2.10 BRUKER 2001'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       block
_exptl_crystal_F_000             991
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_platon_squeeze_details
; 
 Two disordered Ethyl Ether solvent molecules per assymetric unic were 
 squeezed with PLATON (Spek, A. L. (2005). PLATON, A Multipurpose 
 Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands.) 
 Those solvent molecules are, however, included in the reported 
 chemical formula and derived values (e.g. formula weight, F(000), etc) 
;
_refine_diff_density_max         1.251
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.768
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         12638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.768
_refine_ls_R_factor_all          0.2450
_refine_ls_R_factor_gt           0.1006
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0964P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2177
_refine_ls_wR_factor_ref         0.2687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3295
_reflns_number_total             12638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01744d2.cif
_cod_data_source_block           mfcl3_111
_cod_depositor_comments
'Adding full bibliography for 7039416--7039417.cif.'
_cod_database_code               7039417
_shelxl_version_number           2013-3
_shelx_res_checksum              92815
_solvent_exptl_crystal_recrystallization_method 'Diethyl ether, pentane'