Mono-, di- and polymetallic TlI complexes stabilized by a 2,5-bis(2-pyridyl)-1-phenyl-phosphole ligand
Welsch, Stefan; Lescop, Christophe; Réau, Régis; Scheer, Manfred; Dalton Transactions  (2009) 2683–2686; doi:10.1039/b822721g

data_7001003
_publ_section_title
;
 Mono-, di- and polymetallic TlI complexes stabilized by a
 2,5-bis(2-pyridyl)-1-phenyl-phosphole ligand
;
_journal_issue                   15
_journal_name_full               'Dalton Transactions'
_journal_page_first              2683
_journal_page_last               2686
_journal_paper_doi               10.1039/b822721g
_journal_year                    2009
_chemical_compound_source        'see text'
_chemical_formula_moiety
'C16 Al F36 O4, 2(C24 H21 N2 P), Tl, 2(C7 H8)'
_chemical_formula_sum            'C78 H58 Al F36 N4 O4 P2 Tl'
_chemical_formula_weight         2092.58
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 91.045(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6229(1)
_cell_length_b                   23.3032(2)
_cell_length_c                   36.1442(2)
_cell_measurement_reflns_used    28634
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      66.4820
_cell_measurement_theta_min      3.0919
_cell_volume                     8103.79(12)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material
;
PLATON (Spek, 2003) and SHELXH-97 (Sheldrick, 1997)
;
_computing_structure_refinement  'SHELXH-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
1 omega -44.00 12.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -11.6137 71.0000 192.0000 0.0000 0.0000 56

2 omega -13.00 43.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 11.6137 -77.0000 90.0000 0.0000 0.0000 56

3 omega -86.00 -33.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -11.6137 -45.0000 210.0000 0.0000 0.0000 53

4 omega 11.00 61.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -11.6137 45.0000 120.0000 0.0000 0.0000 50

5 omega -166.00 -58.00 1.0000 11.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -90.0000 -71.0000 242.0000 0.0000 0.0000 108

6 omega -115.00 -25.00 1.0000 11.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -90.0000 109.0000 0.0000 0.0000 0.0000 90

7 omega -114.00 -64.00 1.0000 11.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -90.0000 -71.0000 347.0000 0.0000 0.0000 50

8 omega -167.00 -128.00 1.0000 11.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -90.0000 -109.0000 179.0000 0.0000 0.0000 39

9 omega 115.00 171.00 1.0000 11.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 77.0000 210.0000 0.0000 0.0000 56

10 omega 115.00 164.00 1.0000 11.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 45.0000 0.0000 0.0000 0.0000 49

11 omega 92.00 172.00 1.0000 11.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 109.0000 275.0000 0.0000 0.0000 80

12 omega 15.00 82.00 1.0000 11.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -109.0000 359.0000 0.0000 0.0000 67

13 omega 79.00 119.00 1.0000 11.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -45.0000 90.0000 0.0000 0.0000 40

14 omega 77.00 126.00 1.0000 11.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -77.0000 150.0000 0.0000 0.0000 49

;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            33548
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        62.38
_diffrn_reflns_theta_max         62.38
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.541
_exptl_absorpt_correction_T_max  0.355
_exptl_absorpt_correction_T_min  0.286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4136
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.187
_refine_diff_density_max         3.228
_refine_diff_density_min         -1.491
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1566
_refine_ls_number_reflns         12511
_refine_ls_number_restraints     885
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0581P)^2^+58.4966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                11802
_reflns_number_total             12511
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b822721g.txt
_cod_data_source_block           sw139
_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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7001003