Aggregation of thallium(I) beta-diketiminates
Michael Hill; Peter B. Hitchcock; Ruti Pongtavornpinyo; Chemical Communications  (2006) –; doi:10.1039/b607887g

data_7101379
_publ_section_title
;
Aggregation of thallium(I) beta-diketiminates
;
_journal_issue                   35
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b607887g
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C92 H114 N8 O11 Tl8, 2(C6 H14)'
_chemical_formula_sum            'C104 H142 N8 O11 Tl8'
_chemical_formula_weight         3315.22
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-09-30T17:03:28-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.743(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4127(3)
_cell_length_b                   15.1224(3)
_cell_length_c                   29.4433(7)
_cell_measurement_reflns_used    69437
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     5499.1(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.713019E-1
_diffrn_orient_matrix_UB_12      0.5446E-3
_diffrn_orient_matrix_UB_13      0.190991E-1
_diffrn_orient_matrix_UB_21      -0.382836E-1
_diffrn_orient_matrix_UB_22      -0.33471E-2
_diffrn_orient_matrix_UB_23      0.282629E-1
_diffrn_orient_matrix_UB_31      0.25283E-2
_diffrn_orient_matrix_UB_32      -0.660401E-1
_diffrn_orient_matrix_UB_33      -0.1275E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29498
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.73
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    11.733
_exptl_absorpt_correction_T_max  0.8889
_exptl_absorpt_correction_T_min  0.1777
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3116
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.182
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         9534
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+35.5270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                6970
_reflns_number_total             9534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b607887g.txt
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               7101379