(η^8^-Cyclooctatetraene)(2,2'',4,4'',6,6''-hexamethyl-<i>m</i>-terphenyl-κ<i>C</i>^2'^)(tetrahydrofuran-κ<i>O</i>)thulium(III)
Rabe, Gerd W.; Zhang-Preße, Mei; Golen, James A.; Rheingold, Arnold L.; Acta Crystallographica Section E 59 (2003) m1102–m1103; doi:10.1107/S1600536803025005

data_2202729
_publ_section_title
(\h^8^-Cyclooctatetraene)(2,2'',4,4'',6,6''-hexamethyl-<i>m</i>-terphenyl-\k<i>C</i>^2'^)(tetrahydrofuran-\k<i>O</i>)thulium(III)
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1102
_journal_page_last               m1103
_journal_paper_doi               10.1107/S1600536803025005
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Tm (C4 H8 O1) (C8 H8) (C24 H25)]'
_chemical_formula_moiety         'C36 H41 O Tm'
_chemical_formula_sum            'C36 H41 O Tm'
_chemical_formula_weight         658.62
_chemical_name_systematic
;
(\h^8^-Cyclooctatetraenyl)(2,2'',4,4'',6,6''-hexamethyl-\m-
terphenyl-\kC^2'^)(tetrahydrofuran-\kO)thulium(III)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.1317(9)
_cell_length_b                   15.7090(10)
_cell_length_c                   28.594(2)
_cell_measurement_reflns_used    6048
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.47
_cell_volume                     5898.5(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      218(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 4K 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  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            33690
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.034
_exptl_absorpt_correction_T_max  0.8631
_exptl_absorpt_correction_T_min  0.3766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.430
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0334P)^2^+1.0269P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                3903
_reflns_number_total             5203
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6136.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 'Orthorhombic' changed to
'orthorhombic' 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        5898.6(7)
_cod_database_code               2202729
_cod_database_fobs_code          2202729