The Synthesis and Structural Characterization of Polycyclic Derivatives of Cobalt Bis(dicarbollide)(1(-)).
Grüner, Bohumír; Šícha, Václav; Hnyk, Drahomír; Londesborough, Michael G. S.; Císařová, Ivana; Inorganic chemistry 54 (2015) 3148–3158; doi:10.1021/ic502450t

data_4342728
_publ_section_title
;
 The Synthesis and Structural Characterization of Polycyclic Derivatives
 of Cobalt Bis(dicarbollide)(1(-)).
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3148
_journal_page_last               3158
_journal_paper_doi               10.1021/ic502450t
_journal_volume                  54
_journal_year                    2015
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C15 H31 B18 Co N O2, H2 O, Li'
_chemical_formula_sum            'C15 H33 B18 Co Li N O3'
_chemical_formula_weight         535.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.4450(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0702(4)
_cell_length_b                   13.0078(4)
_cell_length_c                   22.9231(9)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.9746
_cell_measurement_theta_min      2.3797
_cell_volume                     3273.1(2)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            47670
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.79
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.9392
_exptl_absorpt_correction_T_min  0.8121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
The rest of coordination sphere of Li atom, as well as voids in the unit cell,
contain unresolvable mixture of solvents (possibly: acetone, water, CHCl2, 
ehter) Therefore application of SQUEEZE was only solution.
;
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+6.5495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1693
_reflns_number_gt                5933
_reflns_number_total             7511
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic502450t_si_001.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4342725--4342728.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4342728