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_4345481
_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         'C20 H30 B Cl2 N8 Ti, C2.5 H3 N'
_chemical_formula_sum            'C22.5 H33 B Cl2 N9 Ti'
_chemical_formula_weight         559.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.57(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.462(4)
_cell_length_b                   10.763(2)
_cell_length_c                   25.135(5)
_cell_volume                     5487.3(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.9501
_diffrn_measured_fraction_theta_max 0.9501
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19049
_diffrn_reflns_theta_full        23.2542
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.536
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.3536
_exptl_crystal_description       Block
_exptl_crystal_F_000             2341.2546
_refine_diff_density_max         0.6120
_refine_diff_density_min         -0.5759
_refine_diff_density_rms         0.1353
_refine_ls_d_res_high            0.9001
_refine_ls_d_res_low             12.4579
_refine_ls_goodness_of_fit_ref   1.0733
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    44
_refine_ls_number_parameters     350
_refine_ls_number_reflns         3735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0733
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.0476
_refine_ls_shift/su_mean         0.0009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+4.5172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                2859
_reflns_number_total             3735
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic6b02643_si_002.cif
_cod_data_source_block           aj002
_cod_original_cell_volume        5488(2)
_cod_database_code               4345481
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C1a(0.5) N9(0.5) N10(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13), C18(H18), C8(H8)
3.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C11(H11a,H11b,H11c),
 C10(H10a,H10b,H10c), C16(H16a,H16b,H16c), C15(H15a,H15b,H15c), C20(H20a,H20b,
 H20c), C21(H21a,H21b,H21c)
;
_olex2_submission_special_instructions 'No special instructions were received'