Improved syntheses, and structural and electronic characterization of carboxamide-substituted Tp^CONHPh,Me^ and Tp^CONH<i>t^-Bu,Me</i> ligands
Sirianni, Eric R.; Yap, Glenn P. A.; Akturk, Eser S.; Theopold, Klaus H.; Acta Crystallographica Section C 69 (2013) 947–953; doi:10.1107/S0108270113015898

data_2019118
_publ_section_title
;
 Improved syntheses, and structural and electronic characterization of
 carboxamide-substituted Tp^CONHPh,Me^ and Tp^CONH<i>t^-Bu,Me</i> ligands
;
_journal_coeditor_code           EG3122
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              947
_journal_page_last               953
_journal_paper_doi               10.1107/S0108270113015898
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Tl (C33 H31 B N9 O3)]'
_chemical_formula_moiety         'C33 H31 B N9 O3 Tl'
_chemical_formula_sum            'C33 H31 B N9 O3 Tl'
_chemical_formula_weight         816.85
_chemical_name_systematic
;
[Tris(3-anilinocarbonyl-5-methylpyrazol-1-yl-\k<i>N</i>^2^)borato]thallium(I)
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_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                   30.2283(4)
_cell_length_b                   30.2283(4)
_cell_length_c                   14.3753(3)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      69.24
_cell_measurement_theta_min      3.40
_cell_volume                     13135.4(4)
_computing_cell_refinement       'APEX2 (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'APEX2 (Bruker, 2007)'
_computing_molecular_graphics    'APEX2 (Bruker, 2007)'
_computing_publication_material  'APEX2 (Bruker, 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 1672
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48743
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         70.13
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    9.854
_exptl_absorpt_correction_T_max  0.6766
_exptl_absorpt_correction_T_min  0.2851
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(APEX2; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6432
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.450
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         6060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0400P)^2^+20.0316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                5178
_reflns_number_total             6060
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3122.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2019118
_cod_database_fobs_code          2019118