{Co(II/III)5} horseshoe and {Ni(II)4} lacunary cubane coordination clusters: the isobutyrate/N-butyldiethanolamine reaction system
Schmitz, Sebastian; Monakhov, Kirill; van Leusen, Jan; Izarova, Natalya V.; Heß, Volkmar; Kögerler, Paul; RSC Adv.  (2016) –; doi:10.1039/C6RA19232G

data_7226819
_publ_section_title
;
 {Co(II/III)5} horseshoe and {Ni(II)4} lacunary cubane coordination
 clusters: the isobutyrate/N-butyldiethanolamine reaction system
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA19232G
_journal_year                    2016
_chemical_formula_sum            'C60 H118 Co5 N6 O20'
_chemical_formula_weight         1538.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-09-22 deposited with the CCDC.
2016-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                96.7233(18)
_cell_angle_beta                 99.379(2)
_cell_angle_gamma                113.656(2)
_cell_formula_units_Z            2
_cell_length_a                   15.2428(4)
_cell_length_b                   16.7140(3)
_cell_length_c                   16.7757(4)
_cell_measurement_reflns_used    12803
_cell_measurement_temperature    119.90(14)
_cell_measurement_theta_max      24.7070
_cell_measurement_theta_min      2.7410
_cell_volume                     3782.91(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0(1)
_diffrn_detector_area_resol_mean 20.9246
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            70202
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         4.08
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.8210
_exptl_absorpt_correction_T_min  0.2364
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1630
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.367
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         13288
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0606P)^2^+8.4205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1607
_reflns_number_gt                8889
_reflns_number_total             13288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra19232g2.cif
_cod_data_source_block           co5-iii
_cod_original_cell_volume        3782.89(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7226819