Titanium(III) Member of the Family of Trigonal Building Blocks with Scorpionate and Cyanide Ligands.
Brown, Andrew; Saber, Mohamed; Van den Heuvel, Willem; Schulte, Kelsey; Soncini, Alessandro; Dunbar, Kim R.; Inorganic chemistry 56 (2017) 1031–1035; doi:10.1021/acs.inorgchem.6b02643

data_4345040
_publ_section_title
;
 Titanium(III) Member of the Family of Trigonal Building Blocks with
 Scorpionate and Cyanide Ligands.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1031
_journal_page_last               1035
_journal_paper_doi               10.1021/acs.inorgchem.6b02643
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C26 H42 B N10 Ti'
_chemical_formula_weight         553.40
_chemical_name_common
'Tetraethylammonium Tricyano[tris(3,5-dimethylpyrazol-1-yl)hydroborate]Titanium(III)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.634(2)
_cell_length_b                   8.1814(16)
_cell_length_c                   15.620(3)
_cell_measurement_reflns_used    3736
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.604
_cell_measurement_theta_min      1.304
_cell_volume                     1486.7(5)
_computing_cell_refinement       'SMART V5.625 (Bruker, 2000)'
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_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17184
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.604
_diffrn_reflns_theta_min         1.304
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.321
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       Block
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 1645 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.013(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3736
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0551P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                3595
_reflns_number_total             3736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02643_si_004.cif
_cod_data_source_block           AJ009A
_cod_depositor_comments          'Adding full bibliography for 4345040.cif.'
_cod_original_cell_volume        1486.8(5)
_cod_database_code               4345040
_shelxl_version_number           2013-3
_shelx_res_checksum              58805
_shelx_hkl_checksum              61998