Crystal structure of an unknown solvate of dodecakis(μ~2~-alaninato-1:2κ^2^<i>O</i>:<i>N</i>,<i>O</i>)cerium(III)hexanickel(II) aquatris(hydroxido-κ<i>O</i>)tris(nitrato-κ^2^<i>O</i>,<i>O</i>')cerate(III)
Bezzubov, Stanislav I.; Doljenko, Vladimir D.; Churakov, Andrei V.; Zharinova, Irina S.; Kiselev, Yuri M.; Acta Crystallographica Section E 71 (2015) m183–m184; doi:10.1107/S2056989015017132

data_2241111
_publ_section_title
;
 Crystal structure of an unknown solvate of
 dodecakis(\m~2~-alaninato-1:2\k^2^<i>O</i>:<i>N</i>,<i>O</i>)cerium(III)hexanickel(II)
 aquatris(hydroxido-\k<i>O</i>)tris(nitrato-\k^2^<i>O</i>,<i>O</i>')cerate(III)
;
_journal_coeditor_code           WM5213
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m183
_journal_page_last               m184
_journal_paper_doi               10.1107/S2056989015017132
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
'[Ce1 Ni6 (C3 H6 N1 O2)12] [Ce (N O3)3 (O H)3 (H2 O)]'
_chemical_formula_moiety         'C36 H72 Ce N12 Ni6 O24 3+, Ce H5 N3 O13 3-'
_chemical_formula_sum            'C36 H77 Ce2 N15 Ni6 O37'
_chemical_formula_weight         1944.63
_chemical_name_systematic
;Dodecakis(\m~2~-alaninato-1:2\k^2^<i>O</i>:<i>N</i>,<i>O</i>)cerium(III)hexanickel(II)
aquatris(hydroxido-\k<i>O</i>)tris(nitrato-\k^2^<i>O</i>,<i>O</i>')cerate(III)
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.6418(4)
_cell_length_b                   14.6418(4)
_cell_length_c                   31.7767(19)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.505
_cell_measurement_theta_min      2.283
_cell_volume                     5899.7(4)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       \w
_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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            21829
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.623
_exptl_absorpt_correction_T_max  0.4201
_exptl_absorpt_correction_T_min  0.4201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2934
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_platon_squeeze_details
;
The refinement using the SQUEEZE procedure resulted in a total potential solvent
accessible void volume of 1020.6 \%A^3^ and an electron count of 437. 12-15
disordered solvent ethanol and 6-9 H2O molecules were removed from the cell.
;
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.686
_refine_ls_abs_structure_details
;
Flack (1983), 3493 Friedel pairs
;
_refine_ls_abs_structure_Flack   -0.012(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         6978
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+4.4547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0655
_reflns_number_gt                6734
_reflns_number_total             6978
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm5213sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        5899.7(6)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               2241111
_cod_database_fobs_code          2241111