Tetrabutylammonium tetrakis(nitrato-κ^2^<i>O,O</i>')[1,3,5-tris(pyrazolyl)methane-κ^3^<i>N</i>]cerate(III)
Chen, Shu-Jian; Li, Yi-Zhi; Chen, Xue-Tai; Shi, Yu-Jun; You, Xiao-Zeng; Acta Crystallographica Section E 58 (2002) m753–m755; doi:10.1107/S1600536802021177

data_2201596
_publ_section_title
;Tetrabutylammonium
 tetrakis(nitrato-\k^2^<i>O,O</i>')[1,3,5-tris(pyrazolyl)methane-\k^3^<i>N</i>]cerate(III)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m753
_journal_page_last               m755
_journal_paper_doi               10.1107/S1600536802021177
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C16 H36 N) [Ce (N O3)4 (C10 H10 N6)]'
_chemical_formula_moiety         'C16 H36 N 1+, C10 H10 Ce N10 O12 1-'
_chemical_formula_sum            'C26 H46 Ce N11 O12'
_chemical_formula_weight         844.86
_chemical_name_systematic
;
Tetrabutylammonium
tetrakis(nitrato-\k^2^O,O')[1,3,5-tris(pyrazolyl)methane-\k^3^N]cerate(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 102.820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4840(10)
_cell_length_b                   16.7420(10)
_cell_length_c                   18.2670(10)
_cell_measurement_reflns_used    4597
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.77
_cell_measurement_theta_min      2.17
_cell_volume                     3722.8(4)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18988
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.293
_exptl_absorpt_correction_T_max  0.771
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 1990)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.590
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0426
_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^)+(0.03P)^2^+1.99P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                4018
_reflns_number_total             6546
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6192.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2201596
_cod_database_fobs_code          2201596