Tl(i) complexes of cymantrene-based tris(1-pyrazolyl)borates: polymers and macrocycles
Guo, ShengLi; Bats, Jan W.; Bolte, Michael; Wagner, Matthias; Journal of the Chemical Society, Dalton Transactions  (2001) 3572–; doi:10.1039/b105692c

data_7702687
_publ_section_title
;
 Tl(i) complexes of cymantrene-based tris(1-pyrazolyl)borates: polymers
 and macrocycles
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3572
_journal_paper_doi               10.1039/b105692c
_journal_year                    2001
_chemical_formula_moiety         'C18 H15 B Mn N6 O3 Tl . (C7 H8)'
_chemical_formula_sum            'C25 H23 B Mn N6 O3 Tl'
_chemical_formula_weight         725.61
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   15.2801(10)
_cell_length_b                   15.2801(10)
_cell_length_c                   45.333(7)
_cell_measurement_reflns_used    322
_cell_measurement_temperature    144(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     10584.4(19)
_computing_cell_refinement       'SMART (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_publication_material  'CIF in SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1996)'
_diffrn_ambient_temperature      144(2)
_diffrn_measurement_device       SIEMENS_SMART
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_sigmaI/netI    0.0683
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            96081
_diffrn_reflns_theta_max         31.61
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  600
_diffrn_standards_number         943
_exptl_absorpt_coefficient_mu    6.597
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.381
_exptl_absorpt_correction_type   'empirical (SADABS, Sheldrick, 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_description       block
_exptl_crystal_F_000             5600
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.24
_refine_ls_extinction_coef       0.00001(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.825
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         8270
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.836
_refine_ls_R_factor_all          0.1703
_refine_ls_R_factor_gt           0.0873
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.06P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1997
_refine_ls_wR_factor_ref         0.2182
_reflns_number_observed          4367
_reflns_number_total             8270
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            b105692c.txt
_cod_data_source_block           compound_2b
_cod_original_cell_volume        10584.5(18)
_cod_original_sg_symbol_H-M      I41/a
_cod_database_code               7702687