[13,27-Dimethyl-3,6,9,17,20,23-hexaazatricyclo[23.3.1.1^11,15^]triaconta-1(29),2,9,11,13,15(30),16,23,25,27-decaene-29,30-diol-κ^5^<i>N</i>^3^,<i>N</i>^6^,<i>N</i>^9^,<i>O</i>^29^,<i>O</i>^30^]bis(nitrato-κ^2^<i>O</i>,<i>O</i>')lutetium(III)–nitrate–water–ethyl acetate (1/1/0.5/0.25)
Hu, Xue-Lei; Chen, Zhong; Qiu, Li; Pan, Zhi-Quan; Acta Crystallographica Section E 63 (2007) m1668–m1669; doi:10.1107/S1600536807022350

data_2213818
_publ_section_title
;[13,27-Dimethyl-3,6,9,17,20,23-hexaazatricyclo[23.3.1.1^11,15^]triaconta-1(29),2,9,11,13,15(30),16,23,25,27-decaene-29,30-diol-\k^5^<i>N</i>^3^,<i>N</i>^6^,<i>N</i>^9^,<i>O</i>^29^,<i>O</i>^30^]bis(nitrato-\k^2^<i>O</i>,<i>O</i>')lutetium(III)--nitrate--water--ethyl
 acetate (1/1/0.5/0.25)
;
_journal_coeditor_code           HG2233
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1668
_journal_page_last               m1669
_journal_paper_doi               10.1107/S1600536807022350
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Lu (C26 H34 N6 O2) (N O3)2] N O3 , 0.5H2 O , 0.25C4 H8 O2'
_chemical_formula_moiety
'C26 H34 Lu N8 O8 + , N1 O3 - , 0.5H2 O , 0.25C4 H8 O2'
_chemical_formula_sum            'C27 H37 Lu N9 O12'
_chemical_formula_weight         854.63
_chemical_name_systematic
;
[13,27-Dimethyl-3,6,9,17,20,23-hexaazatricyclo[23.3.1.1^11,15^]triaconta-
1(29),2,9,11,13,15(30),16,23,25,27-decaene-29,30-diol-
\k^5^N^3^,N^6^,N^9^,O^29^,O^30^]bis(nitrato-\k^2^O,O')lutetium(III)--
nitrate--water--ethyl acetate (1/1/0.5/0.25)
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.307(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.649(3)
_cell_length_b                   14.0182(11)
_cell_length_c                   21.4453(17)
_cell_measurement_reflns_used    5188
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      2.71
_cell_volume                     7239.8(12)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0777
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20514
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.796
_exptl_absorpt_correction_T_max  0.51
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.066
_refine_diff_density_min         -1.577
_refine_ls_abs_structure_details 'Flack (1983), with 2678 Friedel pairs'
_refine_ls_abs_structure_Flack   0.016(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         9791
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.06P)^2^+1.55P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                8284
_reflns_number_total             9791
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2233.cif
_cod_data_source_block           I
_cod_original_cell_volume        7239.8(11)
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum        'C27 H37 Lu1 N9 O12'
_cod_database_code               2213818
_cod_database_fobs_code          2213818