{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_7226820
_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            'C46 H92 N4 Ni4 O16'
_chemical_formula_weight         1192.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   notdet
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-06-27 deposited with the CCDC.
2016-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.09350(14)
_cell_length_b                   19.21243(19)
_cell_length_c                   22.8160(3)
_cell_measurement_reflns_used    16106
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      25.6580
_cell_measurement_theta_min      2.8700
_cell_volume                     5739.55(11)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            58646
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         4.11
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_T_max  0.7546
_exptl_absorpt_correction_T_min  0.4672
_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
multifaceted crystal model
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         11249
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0681P)^2^+7.9287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                9242
_reflns_number_total             11249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra19232g2.cif
_cod_data_source_block           s755
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7226820