Hexakis(antipyrine-<i>O</i>)terbium(III) triperchlorate
Su, Cheng-Yong; Yang, Xiao-Ping; Xu, An-Wu; Zhang, Ze-Fu; Liu, Hong-Ke; Kang, Bei-Sheng; Acta Crystallographica Section C 56 (2000) e82–e83; doi:10.1107/S0108270100002298

data_2010761
_publ_section_title
;
 Hexakis(antipyrine-<i>O</i>)terbium(III) triperchlorate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e82
_journal_page_last               e83
_journal_paper_doi               10.1107/S0108270100002298
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C66 H72 N12 O6 Tb, 3(Cl O4)'
_chemical_formula_sum            'C66 H72 Cl3 N12 O18 Tb'
_chemical_formula_weight         1586.63
_chemical_name_systematic
;
Hexakis(antipyrine-O)terbium(III) triperchlorate
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                   13.9691(10)
_cell_length_b                   13.9691(10)
_cell_length_c                   32.390(3)
_cell_measurement_reflns_used    980
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.8
_cell_measurement_theta_min      2.6
_cell_volume                     5473.7(8)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .998
_diffrn_measured_fraction_theta_max .998
_diffrn_measurement_device_type  'Bruker SMART 1K 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     .71073
_diffrn_reflns_av_R_equivalents  .054
_diffrn_reflns_av_sigmaI/netI    .0439
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            12276
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  .933
_exptl_absorpt_correction_T_min  .793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Multi-scan (Blessing, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2436
_exptl_crystal_size_max          .21
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .06
_refine_diff_density_max         .795
_refine_diff_density_min         -.498
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          .046
_refine_ls_R_factor_gt           .045
_refine_ls_shift/su_max          .017
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0697P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .110
_reflns_number_gt                2688
_reflns_number_total             2800
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qb0180.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5473.6(8)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2010761
_cod_database_fobs_code          2010761