Aquachlorobis(4,4',4''-tri-<i>tert</i>-butyl-2,2';6',2''-terpyridine-κ^3^<i>N</i>)terbium(III) diperchlorate ethanol disolvate
Mürner, Hans-Ruedi; Scopelliti, Rosario; Bünzli, Jean-Claude G.; Acta Crystallographica Section C 58 (2002) m434–m435; doi:10.1107/S0108270102009939

data_2012858
_publ_section_title
;Aquachlorobis(4,4',4''-tri-<i>tert</i>-butyl-2,2';6',2''-terpyridine-\k^3^<i>N</i>)terbium(III)
 diperchlorate ethanol disolvate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m434
_journal_page_last               m435
_journal_paper_doi               10.1107/S0108270102009939
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac
'[Tb (C27 H35 N3)2 Cl (H2 O)] (Cl O4)2 , 2C2 H6 O'
_chemical_formula_moiety         'C54 H72 Cl N6 O Tb 2+ , 2Cl O4 - , 2C2 H6 O'
_chemical_formula_sum            'C58 H84 Cl3 N6 O11 Tb'
_chemical_formula_weight         1306.58
_chemical_name_systematic
;
Aquachlorobis(4,4',4''-tri-tert-butyl-2,2';6',2''-terpyridine-
\k^3^N)terbium(III) diperchlorate ethanol disolvate
;
_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                 106.95(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.392(3)
_cell_length_b                   21.233(4)
_cell_length_c                   22.172(4)
_cell_measurement_reflns_used    708
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      12.23
_cell_measurement_theta_min      1.41
_cell_volume                     6481(2)
_computing_cell_refinement
'marHKL (release 1.9.1), based on HKL (Otwinowski & Minor, 1997)'
_computing_data_collection       'MAR345 Software (marresearch, 19??)'
_computing_data_reduction        marHKL
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'MAR345 IPDS'
_diffrn_measurement_method       '\f scan (\D\f = 3\%; exp. time 180 s)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_sigmaI/netI    0.082
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34863
_diffrn_reflns_theta_full        24.41
_diffrn_reflns_theta_max         24.41
_diffrn_reflns_theta_min         3.24
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.44
_refine_diff_density_min         -1.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         10324
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.112
_refine_ls_R_factor_gt           0.065
_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^)+(0.1083P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.177
_refine_ls_wR_factor_ref         0.203
_reflns_number_gt                5193
_reflns_number_total             10324
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn1012.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2012858
_cod_database_fobs_code          2012858