FcTp(<i>R</i>) (<i>R</i> = ^<i>i^</i>Pr or ^<i>t^</i>Bu): third-generation ferrocenyl scorpionates
Sirianni, Eric R.; Cummins, Daniel C.; Yap, Glenn P. A.; Theopold, Klaus H.; Acta Crystallographica Section C 72 (2016) 813–818; doi:10.1107/S205322961601202X

data_2020617
_publ_section_title
;
 FcTp(<i>R</i>) (<i>R</i> = ^<i>i^</i>Pr or ^<i>t^</i>Bu):
 third-generation ferrocenyl scorpionates
;
_journal_coeditor_code           FO3003
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              813
_journal_page_last               818
_journal_paper_doi               10.1107/S205322961601202X
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Fe Tl (C5 H5) (C23 H31 B N6)]'
_chemical_formula_moiety         'C28 H36 B Fe N6 Tl'
_chemical_formula_sum            'C28 H36 B Fe N6 Tl'
_chemical_formula_weight         727.66
_chemical_name_systematic
;
[Ferrocenyltris(3-isopropylpyrazol-1-yl-\k<i>N</i>^2^)borato]thallium(I)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 97.870(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.4659(9)
_cell_length_b                   15.7392(7)
_cell_length_c                   17.2700(7)
_cell_measurement_reflns_used    5377
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      72.57
_cell_measurement_theta_min      3.49
_cell_volume                     5779.8(4)
_computing_cell_refinement
;
SAINT-PLUS (Bruker, 2006)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT-PLUS (Bruker, 2006)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEXII'
_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  0.1485
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            60805
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         74.48
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    14.813
_exptl_absorpt_correction_T_max  0.4110
_exptl_absorpt_correction_T_min  0.2490
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(APEX2; Bruker, 2006)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.164
_refine_diff_density_min         -2.225
_refine_ls_extinction_coef       0.00018(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   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0922P)^2^+71.9197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1770
_reflns_number_gt                4371
_reflns_number_total             5883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            fo3003sup1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 2020616--2020620.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               2020617
_cod_database_fobs_code          2020617