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_4345480
_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_moiety         'C15 H22 B Cl3 N6 Ti, C8 H20 N'
_chemical_formula_sum            'C23 H42 B Cl3 N7 Ti'
_chemical_formula_weight         581.69
_chemical_name_common
trichloro[tris(3,5-dimethylpyrazolyl)borato]titanate(III)
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-08-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.44(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.669(4)
_cell_length_b                   10.410(2)
_cell_length_c                   17.024(3)
_cell_measurement_reflns_used    3259
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.133
_cell_measurement_theta_min      2.316
_cell_volume                     2914.6(12)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 1.166
_diffrn_measured_fraction_theta_max 1.164
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_unetI/netI     0.1152
_diffrn_reflns_Laue_measured_fraction_full 1.166
_diffrn_reflns_Laue_measured_fraction_max 1.164
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14335
_diffrn_reflns_point_group_measured_fraction_full 1.163
_diffrn_reflns_point_group_measured_fraction_max 1.123
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.570
_diffrn_reflns_theta_min         1.285
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1214 before and 0.0809 after correction. The Ratio of minimum to maximum transmission is 0.7749. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       Block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 1753 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6617
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0932P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1740
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    1.161
_reflns_Friedel_fraction_max     1.082
_reflns_number_gt                4755
_reflns_number_total             6617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02643_si_003.cif
_cod_data_source_block           cc
_cod_database_code               4345480
_shelxl_version_number           2013-3
_shelx_res_checksum              25745
_shelx_hkl_checksum              59551